WorldWideScience

Sample records for acid x-ray crystallography

  1. Nucleic acid X-ray crystallography via direct selenium derivatization.

    Science.gov (United States)

    Lin, Lina; Sheng, Jia; Huang, Zhen

    2011-09-01

    X-ray crystallography has proven to be an essential tool for structural studies of bio-macromolecules at the atomic level. There are two major bottle-neck problems in the macromolecular crystal structure determination: phasing and crystallization. Although the selenium derivatization is routinely used for solving novel protein structures through the MAD phasing technique, the phase problem is still a critical issue in nucleic acid crystallography. The background and current progress of using direct selenium-derivatization of nucleic acids (SeNA) to solve the phase problem and to facilitate nucleic acid crystallization for X-ray crystallography are summarized in this tutorial review. PMID:21666919

  2. X-ray Crystallography Facility

    Science.gov (United States)

    2000-01-01

    Edward Snell, a National Research Council research fellow at NASA's Marshall Space Flight Center (MSFC), prepares a protein crystal for analysis by x-ray crystallography as part of NASA's structural biology program. The small, individual crystals are bombarded with x-rays to produce diffraction patterns, a map of the intensity of the x-rays as they reflect through the crystal.

  3. X-ray crystallography

    Science.gov (United States)

    2001-01-01

    X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

  4. X-ray lasers and crystallography

    OpenAIRE

    Spence, John C. H.

    2014-01-01

    The development of X-ray lasers and their applications in crystallography is described. In the birth of this new field, IUCrJ is ideally positioned to present this research to both specialists in crystallography, and to the wider audience in structural biology.

  5. Synthesis of enantiopure 2-aryl-2-methoxypropionic acids and determination of their absolute configurations by X-ray crystallography.

    Science.gov (United States)

    Sekiguchi, Satoshi; Naito, Junpei; Taji, Hiromi; Kasai, Yusuke; Sugio, Akinori; Kuwahara, Shunsuke; Watanabe, Masataka; Harada, Nobuyuki

    2008-03-01

    Racemic 2-aryl-2-methoxypropionic acids were enantioresolved by the use of (S)-(-)-phenylalaninol 4. For instance, racemic 2-methoxy-2-phenylpropionic acid (+/-)-7 was condensed with phenylalaninol (S)-(-)-4 yielding a diastereomeric mixture of amides, which was easily separated by HPLC on silica gel affording the first-eluted amide (-)-13a and the second-eluted amide (+)-13b: alpha = 3.19, Rs = 3.49. The absolute configuration of amide (-)-13a was determined to be (R;S) by X-ray crystallography by reference to the S configuration of the phenylalaninol moiety. Amide (R;S)-(-)-13a was converted to oxazoline (R;S)-(-)-14a, from which enantiopure 2-methoxy-2-phenylpropionic acid (R)-(-)-7 was recovered. Other 2-aryl-2-methoxypropionic acids, (R)-(-)-8, (R)-(-)-9, (R)-(+)-10, (R)-(-)-11, and (R)-(-)-12, were similarly prepared in enantiopure forms with the use of phenylalaninol (S)-(-)-4, and their absolute configurations were clearly determined by X-ray crystallography or by chemical correlation. PMID:17559106

  6. X-Ray Crystallography Reagent

    Science.gov (United States)

    Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

    2003-01-01

    Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes per square centimeter at the interface. By placing the microcapsules in a high osmotic dewatering solution. the protein solution is gradually made saturated and then supersaturated. and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged. protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D smucture of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

  7. Early days of X-ray crystallography

    CERN Document Server

    Authier, André

    2013-01-01

    This book relates the discovery itself, the early days of X-ray crystallography, and the way the news of the discovery spread round the world. It explains how the first crystal structures were determined, and recounts which were the early applications of X-ray crystallography. It also tells how the concept of space lattice has developed since ancient times, and how our understanding of the nature of light has changed over time. The contributions of the main actors of the story, prior to the discovery, at the time of the discovery and immediately afterwards, are described through their writings and are put into the context of the time, accompanied by brief biographical details.

  8. Structure determination by X-ray crystallography

    CERN Document Server

    Ladd, M F C

    1977-01-01

    Crystallography may be described as the science of the structure of materi­ als, using this word in its widest sense, and its ramifications are apparent over a broad front of current scientific endeavor. It is not surprising, therefore, to find that most universities offer some aspects of crystallography in their undergraduate courses in the physical sciences. It is the principal aim of this book to present an introduction to structure determination by X-ray crystal­ lography that is appropriate mainly to both final-year undergraduate studies in crystallography, chemistry, and chemical physics, and introductory post­ graduate work in this area of crystallography. We believe that the book will be of interest in other disciplines, such as physics, metallurgy, biochemistry, and geology, where crystallography has an important part to play. In the space of one book, it is not possible either to cover all aspects of crystallography or to treat all the subject matter completely rigorously. In particular, certain ...

  9. A glimpse of structural biology through X-ray crystallography.

    Science.gov (United States)

    Shi, Yigong

    2014-11-20

    Since determination of the myoglobin structure in 1957, X-ray crystallography, as the anchoring tool of structural biology, has played an instrumental role in deciphering the secrets of life. Knowledge gained through X-ray crystallography has fundamentally advanced our views on cellular processes and greatly facilitated development of modern medicine. In this brief narrative, I describe my personal understanding of the evolution of structural biology through X-ray crystallography-using as examples mechanistic understanding of protein kinases and integral membrane proteins-and comment on the impact of technological development and outlook of X-ray crystallography.

  10. Structure determination by X-ray crystallography

    CERN Document Server

    Ladd, M F C

    1995-01-01

    X-ray crystallography provides us with the most accurate picture we can get of atomic and molecular structures in crystals. It provides a hard bedrock of structural results in chemistry and in mineralogy. In biology, where the structures are not fully crystalline, it can still provide valuable results and, indeed, the impact here has been revolutionary. It is still an immense field for young workers, and no doubt will provide yet more striking develop­ ments of a major character. It does, however, require a wide range of intellectual application, and a considerable ability in many fields. This book will provide much help. It is a very straightforward and thorough guide to every aspect of the subject. The authors are experienced both as research workers themselves and as teachers of standing, and this is shown in their clarity of exposition. There are plenty of iliustrations and worked examples to aid the student to obtain a real grasp of the subject.

  11. Protein structure validation and analysis with X-ray crystallography.

    Science.gov (United States)

    Papageorgiou, Anastassios C; Mattsson, Jesse

    2014-01-01

    X-ray crystallography is the main technique for the determination of protein structures. About 85 % of all protein structures known to date have been elucidated using X-ray crystallography. Knowledge of the three-dimensional structure of proteins can be used in various applications in biotechnology, biomedicine, drug design, and basic research and as a validation tool for protein modifications, ligand binding, and structural authenticity. Moreover, the requirement for pure, homogeneous, and stable protein solutions in crystallizations makes X-ray crystallography beneficial in other fields of protein research as well. Here, we describe the technique of X-ray protein crystallography and the steps involved for a successful three-dimensional crystal structure determination.

  12. Neutron Nucleic Acid Crystallography.

    Science.gov (United States)

    Chatake, Toshiyuki

    2016-01-01

    The hydration shells surrounding nucleic acids and hydrogen-bonding networks involving water molecules and nucleic acids are essential interactions for the structural stability and function of nucleic acids. Water molecules in the hydration shells influence various conformations of DNA and RNA by specific hydrogen-bonding networks, which often contribute to the chemical reactivity and molecular recognition of nucleic acids. However, X-ray crystallography could not provide a complete description of structural information with respect to hydrogen bonds. Indeed, X-ray crystallography is a powerful tool for determining the locations of water molecules, i.e., the location of the oxygen atom of H2O; however, it is very difficult to determine the orientation of the water molecules, i.e., the orientation of the two hydrogen atoms of H2O, because X-ray scattering from the hydrogen atom is very small.Neutron crystallography is a specialized tool for determining the positions of hydrogen atoms. Neutrons are not diffracted by electrons, but are diffracted by atomic nuclei; accordingly, neutron scattering lengths of hydrogen and its isotopes are comparable to those of non-hydrogen atoms. Therefore, neutron crystallography can determine both of the locations and orientations of water molecules. This chapter describes the current status of neutron nucleic acid crystallographic research as well as the basic principles of neutron diffraction experiments performed on nucleic acid crystals: materials, crystallization, diffraction experiments, and structure determination.

  13. Polycapillary x-ray optics for macromolecular crystallography

    International Nuclear Information System (INIS)

    Polycapillary x-ray optics have found potential application in many different fields, including antiscatter and magnification in mammography, radiography, x-ray fluorescence, x-ray lithography, and x-ray diffraction techniques. In x-ray diffraction, an optic is used to collect divergent x-rays from a point source and redirect them into a quasi-parallel, or slightly focused beam. Monolithic polycapillary optics have been developed recently for macromolecular crystallography and have already shown considerable gains in diffracted beam intensity over pinhole collimation. Development is being pursued through a series of simulations and prototype optics. Many improvements have been made over the stage 1 prototype reported previously, which include better control over the manufacturing process, reducing the diameter of the output beam, and addition of a slight focusing at the output of the optic to further increase x-ray flux at the sample. The authors report the characteristics and performance of the stage 1 and stage 2 optics

  14. The role for an invariant aspartic acid in hypoxanthine phosphoribosyltransferases is examined using saturation mutagenesis, functional analysis, and X-ray crystallography.

    Science.gov (United States)

    Canyuk, B; Focia, P J; Eakin, A E

    2001-03-01

    The role of an invariant aspartic acid (Asp137) in hypoxanthine phosphoribosyltransferases (HPRTs) was examined by site-directed and saturation mutagenesis, functional analysis, and X-ray crystallography using the HPRT from Trypanosoma cruzi. Alanine substitution (D137A) resulted in a 30-fold decrease of k(cat), suggesting that Asp137 participates in catalysis. Saturation mutagenesis was used to generate a library of mutant HPRTs with random substitutions at position 137, and active enzymes were identified by complementation of a bacterial purine auxotroph. Functional analyses of the mutants, including determination of steady-state kinetic parameters and pH-rate dependence, indicate that glutamic acid or glutamine can replace the wild-type aspartate. However, the catalytic efficiency and pH-rate profile for the structural isosteric mutant, D137N, were similar to the D137A mutant. Crystal structures of four of the mutant enzymes were determined in ternary complex with substrate ligands. Structures of the D137E and D137Q mutants reveal potential hydrogen bonds, utilizing several bound water molecules in addition to protein atoms, that position these side chains within hydrogen bond distance of the bound purine analogue, similar in position to the aspartate in the wild-type structure. The crystal structure of the D137N mutant demonstrates that the Asn137 side chain does not form interactions with the purine substrate but instead forms novel interactions that cause the side chain to adopt a nonfunctional rotamer. The results from these structural and functional analyses demonstrate that HPRTs do not require a general base at position 137 for catalysis. Instead, hydrogen bonding sufficiently stabilizes the developing partial positive charge at the N7-atom of the purine substrate in the transition-state to promote catalysis.

  15. A Compact X-Ray System for Macromolecular Crystallography. 5

    Science.gov (United States)

    Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Joy, Marshall

    2000-01-01

    We describe the design and performance of a high flux x-ray system for macromolecular crystallography that combines a microfocus x-ray generator (40 gm FWHM spot size at a power level of 46.5Watts) and a 5.5 mm focal distance polycapillary optic. The Cu K(sub alpha) X-ray flux produced by this optimized system is 7.0 times above the X-ray flux previously reported. The X-ray flux from the microfocus system is also 3.2 times higher than that produced by the rotating anode generator equipped with a long focal distance graded multilayer monochromator (Green optic; CMF24-48-Cu6) and 30% less than that produced by the rotating anode generator with the newest design of graded multilayer monochromator (Blue optic; CMF12-38-Cu6). Both rotating anode generators operate at a power level of 5000 Watts, dissipating more than 100 times the power of our microfocus x-ray system. Diffraction data collected from small test crystals are of high quality. For example, 42,540 reflections collected at ambient temperature from a lysozyme crystal yielded R(sub sym) 5.0% for the data extending to 1.7A, and 4.8% for the complete set of data to 1.85A. The amplitudes of the reflections were used to calculate difference electron density maps that revealed positions of structurally important ions and water molecules in the crystal of lysozyme using the phases calculated from the protein model.

  16. A Compact X-Ray System for Macromolecular Crystallography

    Science.gov (United States)

    Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Gibson, Walter; Joy, Marshall

    2000-01-01

    We describe the design and performance of a high flux x-ray system for a macromolecular crystallography that combines a microfocus x-ray generator (40 micrometer full width at half maximum spot size at a power level of 46.5 W) and a collimating polycapillary optic. The Cu Ka lpha x-ray flux produced by this optimized system through a 500,um diam orifice is 7.0 times greater than the x-ray flux previously reported by Gubarev et al. [M. Gubarev et al., J. Appl. Crystallogr. 33, 882 (2000)]. The x-ray flux from the microfocus system is also 2.6 times higher than that produced by a rotating anode generator equipped with a graded multilayer monochromator (green optic, Osmic Inc. CMF24-48-Cu6) and 40% less than that produced by a rotating anode generator with the newest design of graded multilayer monochromator (blue optic, Osmic, Inc. CMF12-38-Cu6). Both rotating anode generators operate at a power level of 5000 W, dissipating more than 100 times the power of our microfocus x-ray system. Diffraction data collected from small test crystals are of high quality. For example, 42 540 reflections collected at ambient temperature from a lysozyme crystal yielded R(sub sym)=5.0% for data extending to 1.70 A, and 4.8% for the complete set of data to 1.85 A. The amplitudes of the observed reflections were used to calculate difference electron density maps that revealed positions of structurally important ions and water molecules in the crystal of lysozyme using the phases calculated from the protein model.

  17. Sub-atomic resolution X-ray crystallography and neutron crystallography: promise, challenges and potential.

    Science.gov (United States)

    Blakeley, Matthew P; Hasnain, Samar S; Antonyuk, Svetlana V

    2015-07-01

    The International Year of Crystallography saw the number of macromolecular structures deposited in the Protein Data Bank cross the 100000 mark, with more than 90000 of these provided by X-ray crystallography. The number of X-ray structures determined to sub-atomic resolution (i.e. ≤1 Å) has passed 600 and this is likely to continue to grow rapidly with diffraction-limited synchrotron radiation sources such as MAX-IV (Sweden) and Sirius (Brazil) under construction. A dozen X-ray structures have been deposited to ultra-high resolution (i.e. ≤0.7 Å), for which precise electron density can be exploited to obtain charge density and provide information on the bonding character of catalytic or electron transfer sites. Although the development of neutron macromolecular crystallography over the years has been far less pronounced, and its application much less widespread, the availability of new and improved instrumentation, combined with dedicated deuteration facilities, are beginning to transform the field. Of the 83 macromolecular structures deposited with neutron diffraction data, more than half (49/83, 59%) were released since 2010. Sub-mm(3) crystals are now regularly being used for data collection, structures have been determined to atomic resolution for a few small proteins, and much larger unit-cell systems (cell edges >100 Å) are being successfully studied. While some details relating to H-atom positions are tractable with X-ray crystallography at sub-atomic resolution, the mobility of certain H atoms precludes them from being located. In addition, highly polarized H atoms and protons (H(+)) remain invisible with X-rays. Moreover, the majority of X-ray structures are determined from cryo-cooled crystals at 100 K, and, although radiation damage can be strongly controlled, especially since the advent of shutterless fast detectors, and by using limited doses and crystal translation at micro-focus beams, radiation damage can still take place. Neutron

  18. Sub-atomic resolution X-ray crystallography and neutron crystallography: promise, challenges and potential

    Directory of Open Access Journals (Sweden)

    Matthew P. Blakeley

    2015-07-01

    Full Text Available The International Year of Crystallography saw the number of macromolecular structures deposited in the Protein Data Bank cross the 100000 mark, with more than 90000 of these provided by X-ray crystallography. The number of X-ray structures determined to sub-atomic resolution (i.e. ≤1 Å has passed 600 and this is likely to continue to grow rapidly with diffraction-limited synchrotron radiation sources such as MAX-IV (Sweden and Sirius (Brazil under construction. A dozen X-ray structures have been deposited to ultra-high resolution (i.e. ≤0.7 Å, for which precise electron density can be exploited to obtain charge density and provide information on the bonding character of catalytic or electron transfer sites. Although the development of neutron macromolecular crystallography over the years has been far less pronounced, and its application much less widespread, the availability of new and improved instrumentation, combined with dedicated deuteration facilities, are beginning to transform the field. Of the 83 macromolecular structures deposited with neutron diffraction data, more than half (49/83, 59% were released since 2010. Sub-mm3 crystals are now regularly being used for data collection, structures have been determined to atomic resolution for a few small proteins, and much larger unit-cell systems (cell edges >100 Å are being successfully studied. While some details relating to H-atom positions are tractable with X-ray crystallography at sub-atomic resolution, the mobility of certain H atoms precludes them from being located. In addition, highly polarized H atoms and protons (H+ remain invisible with X-rays. Moreover, the majority of X-ray structures are determined from cryo-cooled crystals at 100 K, and, although radiation damage can be strongly controlled, especially since the advent of shutterless fast detectors, and by using limited doses and crystal translation at micro-focus beams, radiation damage can still take place

  19. X-ray detectors for soft X-ray macromolecular crystallography

    International Nuclear Information System (INIS)

    Full text: Modern protein crystallography ultimately makes use of the two-dimensional position - sensitive detectors such as Image Plates and CCD with scintillation convertors coupled with fiber optics for detection of X-Ray diffraction pictures taken from macromolecular crystals. These detectors have high efficiency for 1.5-1.0 A synchrotron radiation, special resolution ∼80-50 μm and large effective area (i.e. Σ 300 mm2 for large MAR Image Plate). Both of these types of detectors lack energy resolution. A major drawback of Image Plates is long read-out time (2.5-4 minutes). CCD based devices permit data collection in a real time, however at present they are much more expensive. One of the novel and very promising trends in protein crystallography is to use soft X-ray synchrotron radiation between 2.2 keV and 6 keV (5.6 to 2.5 A) and there is an urgent need to develop suitable detection system for these kinds of applications. It is to be two- dimensional positional sensitive detector with pitch of about 10 to 20 μm, high efficiency and real-time readout. An active area of the detector is to be at least 20 x 20 mm2. It seems to be the simplest solution to use conventional direct-illumination CCD detectors because absorption length of the 5 A radiation in silicon is about 3 μm. However they lack, for example, energy resolution and optimum solution of the problem has yet to come. (author)

  20. Metalloprotein active site structure determination: synergy between X-ray absorption spectroscopy and X-ray crystallography.

    Science.gov (United States)

    Cotelesage, Julien J H; Pushie, M Jake; Grochulski, Pawel; Pickering, Ingrid J; George, Graham N

    2012-10-01

    Structures of metalloprotein active sites derived from X-ray crystallography frequently contain chemical anomalies such as unexpected atomic geometries or elongated bond-lengths. Such anomalies are expected from the known errors inherent in macromolecular crystallography (ca. 0.1-0.2Å) and from the lack of appropriate restraints for metal sites which are often without precedent in the small molecule structure literature. Here we review the potential of X-ray absorption spectroscopy to provide information and perspective which could aid in improving the accuracy of metalloprotein crystal structure solutions. We also review the potential problem areas in analysis of the extended X-ray absorption fine structure (EXAFS) and discuss the use of density functional theory as another possible source of geometrical restraints for crystal structure analysis of metalloprotein active sites.

  1. X-ray crystallography over the past decade for novel drug discovery – where are we heading next?

    Science.gov (United States)

    Zheng, Heping; Handing, Katarzyna B; Zimmerman, Matthew D; Shabalin, Ivan G; Almo, Steven C; Minor, Wladek

    2015-01-01

    Introduction Macromolecular X-ray crystallography has been the primary methodology for determining the three-dimensional structures of proteins, nucleic acids and viruses. Structural information has paved the way for structure-guided drug discovery and laid the foundations for structural bioinformatics. However, X-ray crystallography still has a few fundamental limitations, some of which may be overcome and complemented using emerging methods and technologies in other areas of structural biology. Areas covered This review describes how structural knowledge gained from X-ray crystallography has been used to advance other biophysical methods for structure determination (and vice versa). This article also covers current practices for integrating data generated by other biochemical and biophysical methods with those obtained from X-ray crystallography. Finally, the authors articulate their vision about how a combination of structural and biochemical/biophysical methods may improve our understanding of biological processes and interactions. Expert opinion X-ray crystallography has been, and will continue to serve as, the central source of experimental structural biology data used in the discovery of new drugs. However, other structural biology techniques are useful not only to overcome the major limitation of X-ray crystallography, but also to provide complementary structural data that is useful in drug discovery. The use of recent advancements in biochemical, spectroscopy and bioinformatics methods may revolutionize drug discovery, albeit only when these data are combined and analyzed with effective data management systems. Accurate and complete data management is crucial for developing experimental procedures that are robust and reproducible. PMID:26177814

  2. Crystals x-rays and proteins comprehensive protein crystallography

    CERN Document Server

    Sherwood, Dennis

    2011-01-01

    Information derived from X-ray crystal structures of biological molecules allows us to explain their functions in living organisms and to develop drugs to treat disease. This book describes the principles and practice of X-ray diffraction as a key technique at the forefront of new discoveries in biology and medicine.

  3. X-Ray Crystallography: One Century of Nobel Prizes

    Science.gov (United States)

    Galli, Simona

    2014-01-01

    In 2012, the United Nations General Assembly declared 2014 the International Year of Crystallography. Throughout the year 2014 and beyond, all the crystallographic associations and societies active all over the world are organizing events to attract the wider public toward crystallography and the numerous topics to which it is deeply interlinked.…

  4. A Compact X-Ray System for Support of High Throughput Crystallography

    Science.gov (United States)

    Ciszak, Ewa; Gubarev, Mikhail; Gibson, Walter M.; Joy, Marshall K.; Whitaker, Ann F. (Technical Monitor)

    2001-01-01

    Standard x-ray systems for crystallography rely on massive generators coupled with optics that guide X-ray beams onto the crystal sample. Optics for single-crystal diffractometry include total reflection mirrors, polycapillary optics or graded multilayer monochromators. The benefit of using polycapillary optic is that it can collect x-rays over tile greatest solid angle, and thus most efficiently, utilize the greatest portion of X-rays emitted from the Source, The x-ray generator has to have a small anode spot, and thus its size and power requirements can be substantially reduced We present the design and results from the first high flux x-ray system for crystallography that combine's a microfocus X-ray generator (40microns FWHM Spot size at a power of 45 W) and a collimating, polycapillary optic. Diffraction data collected from small test crystals with cell dimensions up to 160A (lysozyme and thaumatin) are of high quality. For example, diffraction data collected from a lysozyme crystal at RT yielded R=5.0% for data extending to 1.70A. We compare these results with measurements taken from standard crystallographic systems. Our current microfocus X-ray diffraction system is attractive for supporting crystal growth research in the standard crystallography laboratory as well as in remote, automated crystal growth laboratory. Its small volume, light-weight, and low power requirements are sufficient to have it installed in unique environments, i.e.. on-board International Space Station.

  5. X-ray diffraction and the beginnings of X-ray crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Juretschke, H.J. [Polytechnic Univ., Brooklyn, NY (United States)

    1995-12-31

    A retelling of the discovery of X-ray diffraction in Munich in 1912, and an overview of its rapidity spreading applications to crystal structure determination. The early work by Laue`s group and by approaches and different instrumentation, soon set two basic patterns of investigations in this field, with Ewald offering a grand theoretical framework for encompassing both. Some of the successes, problems, and interplays of these trends are reviewed, also as reflected in the stimulation and response by other early participants in structural research, as well as by the interruptions caused by the first World War.

  6. Apparatus and method for nanoflow liquid jet and serial femtosecond x-ray protein crystallography

    Science.gov (United States)

    Bogan, Michael J.; Laksmono, Hartawan; Sierra, Raymond G.

    2016-03-01

    Techniques for nanoflow serial femtosecond x-ray protein crystallography include providing a sample fluid by mixing a plurality of a first target of interest with a carrier fluid and injecting the sample fluid into a vacuum chamber at a rate less than about 4 microliters per minute. In some embodiments, the carrier fluid has a viscosity greater than about 3 centipoise.

  7. Structural investigation of bistrifluron using x-ray crystallography, NMR spectroscopy, and molecular modeling

    CERN Document Server

    Moon, J K; Rhee, S K; Kim, G B; Yun, H S; Chung, B J; Lee, S S; Lim, Y H

    2002-01-01

    A new insecticide, bistrifluron acts as an inhibitor of insect development and interferes with the cuticle formation of insects. Since it shows low acute oral and dermal toxicities, it can be one of potent insecticides. Based on X-ray crystallography, NMR spectroscopy and molecular modeling, the structural studies of bistrifluron have been carried out.

  8. First Results from a Microfocus X-Ray System for Macromolecular Crystallography

    Science.gov (United States)

    Gubarev, Mikhail; Ciszak, Ewa; Ponomarev, Igor; Gibson, Walter; Joy, Marshall

    1999-01-01

    The design and performance of a 40 Watt laboratory crystallography system optimized for the structure determination of small protein crystals are described. This system combines a microfocus x-ray generator (40 microns FWHM spot size at a power level of 40 Watts) and a short focal length (F = 2.6 mm) polycapillary collimating optic, and produces a small diameter quasi-parallel x-ray beam. Measurements of x-ray flux, divergence and spectral purity of the resulting x-ray beam are presented. The x-ray flux in a 250 microns diameter aperture produced by the microfocus system is 14.7 times higher .than that from a 3.15 kW rotating anode generator equipped with graphite monochromator. Crystallography data taken with the microfocus system are presented, and indicate that the divergence and spectral purity of the x-ray are sufficient to refine the diffraction data using a standard crystallographic software. Significant additional improvements in flux and beam divergence are possible, and plans for achieving these coals are discussed.

  9. SPINE-compatible `carboloops': a new microshaped vitreous carbon sample mount for X-ray and neutron crystallography.

    Science.gov (United States)

    Romoli, Filippo; Mossou, Estelle; Cuypers, Maxime; van der Linden, Peter; Carpentier, Philippe; Mason, Sax A; Forsyth, V Trevor; McSweeney, Sean

    2014-05-01

    A novel vitreous carbon mount for macromolecular crystallography, suitable for neutron and X-ray crystallographic studies, has been developed. The technology described here is compatible both with X-ray and neutron cryo-crystallography. The mounts have low density and low background scattering for both neutrons and X-rays. They are prepared by laser cutting, allowing high standards of production quality, the ability to custom-design the mount to specific crystal sizes and large-scale production.

  10. Visualization of X-ray Beam Using CdWO4 Crystal for Macromolecular Crystallography

    Directory of Open Access Journals (Sweden)

    Kazimierz J. Gofron

    2011-12-01

    Full Text Available In synchrotron diffraction experiments, it is typically assumed that the X-ray beam at the sample position is uniform, stable and has dimensions that are controlled by the focus and slits settings. As might be expected, this process is much more complex. We present here an investigation of the properties of a synchrotron X-ray beam at the sample position. The X-ray beam is visualized with a single crystal scintillator that converts X-ray photons into visible light photons, which can be imaged using Structure Biology Center (SBC on-axis and off-axis microscope optics. The X-ray penetration is dependent on the composition of the scintillator (especially the effective Z, and X-ray energy. Several scintillators have been used to visualize X-ray beams. Here we compare CdWO4, PbWO4, Bi4Ge3O12, Y3Al5O12:Ce (YAG:Ce, and Gd2O2S:Tb (phosphor. We determined that scintillator crystals made of CdWO4 and similar high-Z materials are best suited for the energy range (7–20 keV and are most suitable for beam visualization for macromolecular crystallography applications. These scintillators show excellent absorption, optical, and mechanical properties.

  11. 100 Years later: Celebrating the contributions of x-ray crystallography to allergy and clinical immunology.

    Science.gov (United States)

    Pomés, Anna; Chruszcz, Maksymilian; Gustchina, Alla; Minor, Wladek; Mueller, Geoffrey A; Pedersen, Lars C; Wlodawer, Alexander; Chapman, Martin D

    2015-07-01

    Current knowledge of molecules involved in immunology and allergic disease results from the significant contributions of x-ray crystallography, a discipline that just celebrated its 100th anniversary. The histories of allergens and x-ray crystallography are intimately intertwined. The first enzyme structure to be determined was lysozyme, also known as the chicken food allergen Gal d 4. Crystallography determines the exact 3-dimensional positions of atoms in molecules. Structures of molecular complexes in the disciplines of immunology and allergy have revealed the atoms involved in molecular interactions and mechanisms of disease. These complexes include peptides presented by MHC class II molecules, cytokines bound to their receptors, allergen-antibody complexes, and innate immune receptors with their ligands. The information derived from crystallographic studies provides insights into the function of molecules. Allergen function is one of the determinants of environmental exposure, which is essential for IgE sensitization. Proteolytic activity of allergens or their capacity to bind LPSs can also contribute to allergenicity. The atomic positions define the molecular surface that is accessible to antibodies. In turn, this surface determines antibody specificity and cross-reactivity, which are important factors for the selection of allergen panels used for molecular diagnosis and the interpretation of clinical symptoms. This review celebrates the contributions of x-ray crystallography to clinical immunology and allergy, focusing on new molecular perspectives that influence the diagnosis and treatment of allergic diseases.

  12. Towards an integrative structural biology approach: combining Cryo-TEM, X-ray crystallography, and NMR.

    Science.gov (United States)

    Lengyel, Jeffrey; Hnath, Eric; Storms, Marc; Wohlfarth, Thomas

    2014-09-01

    Cryo-transmission electron microscopy (Cryo-TEM) and particularly single particle analysis is rapidly becoming the premier method for determining the three-dimensional structure of protein complexes, and viruses. In the last several years there have been dramatic technological improvements in Cryo-TEM, such as advancements in automation and use of improved detectors, as well as improved image processing techniques. While Cryo-TEM was once thought of as a low resolution structural technique, the method is currently capable of generating nearly atomic resolution structures on a routine basis. Moreover, the combination of Cryo-TEM and other methods such as X-ray crystallography, nuclear magnetic resonance spectroscopy, and molecular dynamics modeling are allowing researchers to address scientific questions previously thought intractable. Future technological developments are widely believed to further enhance the method and it is not inconceivable that Cryo-TEM could become as routine as X-ray crystallography for protein structure determination.

  13. X-ray crystallography and its impact on understanding bacterial cell wall remodeling processes.

    Science.gov (United States)

    Büttner, Felix Michael; Renner-Schneck, Michaela; Stehle, Thilo

    2015-02-01

    The molecular structure of matter defines its properties and function. This is especially true for biological macromolecules such as proteins, which participate in virtually all biochemical processes. A three dimensional structural model of a protein is thus essential for the detailed understanding of its physiological function and the characterization of essential properties such as ligand binding and reaction mechanism. X-ray crystallography is a well-established technique that has been used for many years, but it is still by far the most widely used method for structure determination. A particular strength of this technique is the elucidation of atomic details of molecular interactions, thus providing an invaluable tool for a multitude of scientific projects ranging from the structural classification of macromolecules over the validation of enzymatic mechanisms or the understanding of host-pathogen interactions to structure-guided drug design. In the first part of this review, we describe essential methodological and practical aspects of X-ray crystallography. We provide some pointers that should allow researchers without a background in structural biology to assess the overall quality and reliability of a crystal structure. To highlight its potential, we then survey the impact X-ray crystallography has had on advancing an understanding of a class of enzymes that modify the bacterial cell wall. A substantial number of different bacterial amidase structures have been solved, mostly by X-ray crystallography. Comparison of these structures highlights conserved as well as divergent features. In combination with functional analyses, structural information on these enzymes has therefore proven to be a valuable template not only for understanding their mechanism of catalysis, but also for targeted interference with substrate binding.

  14. Time-resolved protein nano-crystallography using an X-ray free-electron laser

    International Nuclear Information System (INIS)

    We demonstrate the use of an X-ray free electron laser synchronized with an optical pump laser to obtain X-ray diffraction snapshots from the photo-activated states of large membrane protein complexes in the form of nano-crystals flowing in a liquid jet. Light-induced changes of Photosystem I-Ferredoxin co-crystals were observed at time delays of 5 to 10 μs after excitation. The result correlates with the microsecond kinetics of electron transfer from Photosystem I to ferredoxin. The undocking process that follows the electron transfer leads to large rearrangements in the crystals that will terminally lead to the disintegration of the crystals. We describe the experimental setup and obtain the first time resolved femtosecond serial X-ray crystallography results from an irreversible photo-chemical reaction at the Linac Coherent Light Source. This technique opens the door to time-resolved structural studies of reaction dynamics in biological systems. (authors)

  15. Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature.

    Science.gov (United States)

    Tsujino, Soichiro; Tomizaki, Takashi

    2016-01-01

    Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinning of the crystal within a levitating droplet ensured an efficient sampling of the reciprocal space. The datasets were processed with a program suite developed for serial femtosecond crystallography (SFX). The structure, which was solved by molecular replacement, was found to be identical to the structure obtained by the conventional oscillation method for up to a 1.8-Å resolution limit. In particular, the absence of protein crystal damage resulting from the acoustic levitation was carefully established. These results represent a key step towards a fully automated sample handling and measurement pipeline, which has promising prospects for a high acquisition rate and high sample efficiency for room temperature X-ray crystallography. PMID:27150272

  16. The Mn₄Ca photosynthetic water-oxidation catalyst studied by simultaneous X-ray spectroscopy and crystallography using an X-ray free-electron laser.

    Science.gov (United States)

    Tran, Rosalie; Kern, Jan; Hattne, Johan; Koroidov, Sergey; Hellmich, Julia; Alonso-Mori, Roberto; Sauter, Nicholas K; Bergmann, Uwe; Messinger, Johannes; Zouni, Athina; Yano, Junko; Yachandra, Vittal K

    2014-07-17

    The structure of photosystem II and the catalytic intermediate states of the Mn₄CaO₅ cluster involved in water oxidation have been studied intensively over the past several years. An understanding of the sequential chemistry of light absorption and the mechanism of water oxidation, however, requires a new approach beyond the conventional steady-state crystallography and X-ray spectroscopy at cryogenic temperatures. In this report, we present the preliminary progress using an X-ray free-electron laser to determine simultaneously the light-induced protein dynamics via crystallography and the local chemistry that occurs at the catalytic centre using X-ray spectroscopy under functional conditions at room temperature.

  17. Mapping the continuous reciprocal space intensity distribution of X-ray serial crystallography.

    Science.gov (United States)

    Yefanov, Oleksandr; Gati, Cornelius; Bourenkov, Gleb; Kirian, Richard A; White, Thomas A; Spence, John C H; Chapman, Henry N; Barty, Anton

    2014-07-17

    Serial crystallography using X-ray free-electron lasers enables the collection of tens of thousands of measurements from an equal number of individual crystals, each of which can be smaller than 1 µm in size. This manuscript describes an alternative way of handling diffraction data recorded by serial femtosecond crystallography, by mapping the diffracted intensities into three-dimensional reciprocal space rather than integrating each image in two dimensions as in the classical approach. We call this procedure 'three-dimensional merging'. This procedure retains information about asymmetry in Bragg peaks and diffracted intensities between Bragg spots. This intensity distribution can be used to extract reflection intensities for structure determination and opens up novel avenues for post-refinement, while observed intensity between Bragg peaks and peak asymmetry are of potential use in novel direct phasing strategies.

  18. Mapping the continuous reciprocal space intensity distribution of X-ray serial crystallography.

    Science.gov (United States)

    Yefanov, Oleksandr; Gati, Cornelius; Bourenkov, Gleb; Kirian, Richard A; White, Thomas A; Spence, John C H; Chapman, Henry N; Barty, Anton

    2014-07-17

    Serial crystallography using X-ray free-electron lasers enables the collection of tens of thousands of measurements from an equal number of individual crystals, each of which can be smaller than 1 µm in size. This manuscript describes an alternative way of handling diffraction data recorded by serial femtosecond crystallography, by mapping the diffracted intensities into three-dimensional reciprocal space rather than integrating each image in two dimensions as in the classical approach. We call this procedure 'three-dimensional merging'. This procedure retains information about asymmetry in Bragg peaks and diffracted intensities between Bragg spots. This intensity distribution can be used to extract reflection intensities for structure determination and opens up novel avenues for post-refinement, while observed intensity between Bragg peaks and peak asymmetry are of potential use in novel direct phasing strategies. PMID:24914160

  19. Analysis of urinary stone composition in Eastern India by X-ray diffraction crystallography

    Directory of Open Access Journals (Sweden)

    Tarun Jindal

    2014-01-01

    Full Text Available Background: Stones in the urinary system are common in our country. This study was done to assess the composition of the urinary stones in eastern part of India. Materials and Methods: A prospective study was done over a period of thirty months. A total of 90 stones were analyzed in this time period by using X-ray diffraction crystallography. Results: Of the 90 stones analyzed, 77 were renal stones, 12 were ureteric stones and one was a bladder stone. Six stones (all renal did not have properties to be represented by X-ray diffraction crystallography. The overall prevalence of the oxalate containing stones was 85.7% with calcium oxalate monohydrate (COM being the major constituent. Calcium oxalate dihydrate (COD was the next most common constituent. Struvite stones constituted 9.5% of the stones analyzed. Pure calcium phosphate stones were found in 4.7% of the cases. Conclusion: Our study reveals that the stone composition in the eastern part of India is different from that in other parts of the country. We have a comparatively lower prevalence of oxalate stones while a higher prevalence of phosphate and struvite stones.

  20. In meso in situ serial X-ray crystallography of soluble and membrane proteins

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Chia-Ying [Trinity College, Dublin (Ireland); Olieric, Vincent [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Ma, Pikyee [Trinity College, Dublin (Ireland); Panepucci, Ezequiel [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Diederichs, Kay [Universität Konstanz, M647, D-78457 Konstanz (Germany); Wang, Meitian, E-mail: meitian.wang@psi.ch [Paul Scherrer Institute, CH-5232 Villigen (Switzerland); Caffrey, Martin, E-mail: meitian.wang@psi.ch [Trinity College, Dublin (Ireland)

    2015-05-14

    A method for performing high-throughput in situ serial X-ray crystallography with soluble and membrane proteins in the lipid cubic phase is described. It works with microgram quantities of protein and lipid (and ligand when present) and is compatible with the most demanding sulfur SAD phasing. The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β{sub 2}-adrenoreceptor–G{sub s} protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at

  1. Splendid Century of X-ray Crystallography%X射线晶体学的百年辉煌

    Institute of Scientific and Technical Information of China (English)

    马礼敦

    2014-01-01

    It has been more than one century since Max von Laue discovered the X-ray diffraction by copper sulfate crystal and W. L. Bragg pioneered the X-ray Crystallography. This has been one of the major milestones in the progress of modern sciences, in particular in the sciences and technologies of microstructures. In the past 100 years, the X-ray Crystallography has developed rapidly with significant scientific achievements. In this review article, the history of the X-ray Crystallography is highlighted from four distinct stages for the X-ray crystallographic experimental techniques. In each of the ma jor stages, the developments of the X-ray Crystallography in terms of the sin-gle crystal diffraction, powder diffraction, and X-ray spectroscopy are presented. Furthermore, the profound impacts of the X-ray Crystallography on not only basic sciences such as Physics, Crystallography, Chemistry and Biology, but also applied sciences such as Materials, Medicine, Pharmacology, Environments and so on, are described. The future challenges and opportuni-ties for the X-ray Crystallography, including several scientific frontiers such as the giant X-ray source-hard X-ray free electron laser, multi-dimensional crystallography, electron crystallography, mathematical crystallography, and three-dimensional X-ray diffraction microscopy etc will be dis-cussed. It is believed that as much as has been achieved in the last century, even more will be expected in the next 100 years.%自1912年劳厄发现X射线晶体衍射现象,小布拉格开创X射线晶体学以来,已经过去了100年。这一发现,对人类科学的发展,特别是微观结构科学的影响至为巨大,具有里程碑的意义。在这100年中,X射线晶体学发展迅速,成果累累。本文按主要实验技术的特点将100年大致分为四个阶段,从单晶体衍射、多晶体衍射和X射线光谱三个方面简述其主要进展和成果。并简单概括了她对物理学、晶体学、

  2. In meso in situ serial X-ray crystallography of soluble and membrane proteins.

    Science.gov (United States)

    Huang, Chia Ying; Olieric, Vincent; Ma, Pikyee; Panepucci, Ezequiel; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

    2015-06-01

    The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β2-adrenoreceptor-Gs protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular crystallography synchrotron beamlines worldwide. Because of its simplicity and effectiveness, the IMISX approach is likely to supplant existing in meso crystallization protocols. It should prove particularly attractive in the area of ligand screening for drug discovery and development.

  3. NATO Advanced Study Institute on Chemical Crystallography with Pulsed Neutrons and Synchrotron X-Rays

    CERN Document Server

    Jeffrey, George

    1988-01-01

    X-ray and neutron crystallography have played an increasingly impor­ tant role in the chemical and biochemical sciences over the past fifty years. The principal obstacles in this methodology, the phase problem and com­ puting, have been overcome. The former by the methods developed in the 1960's and just recognised by the 1985 Chemistry Nobel Prize award to Karle and Hauptman, the latter by the dramatic advances that have taken place in computer technology in the past twenty years. Within the last decade, two new radiation sources have been added to the crystallographer's tools. One is synchrotron X-rays and the other is spallation neutrons. Both have much more powerful fluxes than the pre­ vious sources and they are pulsed rather than continuos. New techniques are necessary to fully exploit the intense continuos radiation spectrum and its pulsed property. Both radiations are only available from particular National Laboratories on a guest-user basis for scientists outside these Na­ tional Laboratories. Hi...

  4. The need for a shared database infrastructure: combining X-ray crystallography and electron microscopy

    International Nuclear Information System (INIS)

    Advances in structural biology are opening greater opportunities for understanding biological structures from the cellular to the atomic level. Particularly promising are the links that can be established between the information provided by electron microscopy and the atomic structures derived from X-ray crystallography and nuclear magnetic resonance spectroscopy. Combining such different kinds of structural data can result in novel biological information on the interaction of biomolecules in large supramolecular assemblies. As a consequence, the need to develop new databases in the field of structural biology that allow for an integrated access to data from all the experimental techniques is becoming critical. Pilot studies performed in recent years have already established a solid background as far as the basic information that an integrated macromolecular structure database should contain, as well as the basic principles for integration. These efforts started in the context of the BioImage project, and resulted in a first complete database prototype that provided a versatile platform for the linking of atomic models of X-ray diffraction data with electron microscopy information. Analysis of the requirements needed to combine data at different levels of resolution have resulted in sets of specifications that make possible the integration of all these different types in the context of a web environment. The case of a structural study linking electron microscopy and X-ray data, which is already contained within the BioImage data base and in the Protein Data Bank, is used here to illustrate the current approach, while a general discussion highlights the urgent need for integrated databases. (orig.)

  5. X-ray crystallography: Assessment and validation of protein-small molecule complexes for drug discovery

    Science.gov (United States)

    Cooper, David R.; Porebski, Przemyslaw J.; Chruszcz, Maksymilian; Minor, Wladek

    2011-01-01

    Introduction Crystallography is the key initial component for structure-based and fragment-based drug design and can often generate leads that can be developed into high potency drugs. Therefore, huge sums of money are committed based on the outcome of crystallography experiments and their interpretation. Areas covered This review discusses how to evaluate the correctness of an X-ray structure, focusing on the validation of small molecule-protein complexes. Various types of inaccuracies found within the PDB are identified and the ramifications of these errors are discussed. The reader will gain an understanding of the key parameters that need to be inspected before a structure can be used in drug discovery efforts, as well as an appreciation of the difficulties of correctly interpreting electron density for small molecules. The reader will also be introduced to methods for validating small molecules within the context of a macromolecular structure. Expert opinion One of the reasons that ligand identification and positioning, within a macromolecular crystal structure, is so difficult is that the quality of small molecules widely varies in the PDB. For this reason, the PDB can not always be considered a reliable repository of structural information pertaining to small molecules, and this makes the derivation of general principles that govern small molecule-protein interactions more difficult. PMID:21779303

  6. NATURAL CYCLOPENTANOID CYANOHYDRIN GLYCOSIDES .13. STRUCTURE DETERMINATION OF NATURAL EPOXYCYCLOPENTANES BY X-RAY CRYSTALLOGRAPHY AND NMR-SPECTROSCOPY

    DEFF Research Database (Denmark)

    Olafsdottir, E. S.; Sorensen, A. M.; Cornett, Claus;

    1991-01-01

    nonannellated cyclopentane derivatives. The new glucosides were shown, by NMR spectroscopy (including NOE measurements), X-ray crystallography, and enzymatic hydrolysis to the corresponding cyanohydrins, to be (1R,2R,3R,4R)- and (1S,2S,3S,4S)-1-(beta-D-glucopyranosyloxy)-2,3-epoxy-4-hydroxycyclopenta ne-1...

  7. In vivo crystallography at X-ray free-electron lasers: the next generation of structural biology?

    Science.gov (United States)

    Gallat, François-Xavier; Matsugaki, Naohiro; Coussens, Nathan P; Yagi, Koichiro J; Boudes, Marion; Higashi, Tetsuya; Tsuji, Daisuke; Tatano, Yutaka; Suzuki, Mamoru; Mizohata, Eiichi; Tono, Kensuke; Joti, Yasumasa; Kameshima, Takashi; Park, Jaehyun; Song, Changyong; Hatsui, Takaki; Yabashi, Makina; Nango, Eriko; Itoh, Kohji; Coulibaly, Fasséli; Tobe, Stephen; Ramaswamy, S; Stay, Barbara; Iwata, So; Chavas, Leonard M G

    2014-07-17

    The serendipitous discovery of the spontaneous growth of protein crystals inside cells has opened the field of crystallography to chemically unmodified samples directly available from their natural environment. On the one hand, through in vivo crystallography, protocols for protein crystal preparation can be highly simplified, although the technique suffers from difficulties in sampling, particularly in the extraction of the crystals from the cells partly due to their small sizes. On the other hand, the extremely intense X-ray pulses emerging from X-ray free-electron laser (XFEL) sources, along with the appearance of serial femtosecond crystallography (SFX) is a milestone for radiation damage-free protein structural studies but requires micrometre-size crystals. The combination of SFX with in vivo crystallography has the potential to boost the applicability of these techniques, eventually bringing the field to the point where in vitro sample manipulations will no longer be required, and direct imaging of the crystals from within the cells will be achievable. To fully appreciate the diverse aspects of sample characterization, handling and analysis, SFX experiments at the Japanese SPring-8 angstrom compact free-electron laser were scheduled on various types of in vivo grown crystals. The first experiments have demonstrated the feasibility of the approach and suggest that future in vivo crystallography applications at XFELs will be another alternative to nano-crystallography.

  8. Developing advanced X-ray scattering methods combined with crystallography and computation.

    Science.gov (United States)

    Perry, J Jefferson P; Tainer, John A

    2013-03-01

    The extensive use of small angle X-ray scattering (SAXS) over the last few years is rapidly providing new insights into protein interactions, complex formation and conformational states in solution. This SAXS methodology allows for detailed biophysical quantification of samples of interest. Initial analyses provide a judgment of sample quality, revealing the potential presence of aggregation, the overall extent of folding or disorder, the radius of gyration, maximum particle dimensions and oligomerization state. Structural characterizations include ab initio approaches from SAXS data alone, and when combined with previously determined crystal/NMR, atomistic modeling can further enhance structural solutions and assess validity. This combination can provide definitions of architectures, spatial organizations of protein domains within a complex, including those not determined by crystallography or NMR, as well as defining key conformational states of a protein interaction. SAXS is not generally constrained by macromolecule size, and the rapid collection of data in a 96-well plate format provides methods to screen sample conditions. This includes screening for co-factors, substrates, differing protein or nucleotide partners or small molecule inhibitors, to more fully characterize the variations within assembly states and key conformational changes. Such analyses may be useful for screening constructs and conditions to determine those most likely to promote crystal growth of a complex under study. Moreover, these high throughput structural determinations can be leveraged to define how polymorphisms affect assembly formations and activities. This is in addition to potentially providing architectural characterizations of complexes and interactions for systems biology-based research, and distinctions in assemblies and interactions in comparative genomics. Thus, SAXS combined with crystallography/NMR and computation provides a unique set of tools that should be considered

  9. Life in the fast lane for protein crystallization and X-ray crystallography

    Science.gov (United States)

    Pusey, Marc L.; Liu, Zhi-Jie; Tempel, Wolfram; Praissman, Jeremy; Lin, Dawei; Wang, Bi-Cheng; Gavira, Jose A.; Ng, Joseph D.

    2005-01-01

    The common goal for structural genomic centers and consortiums is to decipher as quickly as possible the three-dimensional structures for a multitude of recombinant proteins derived from known genomic sequences. Since X-ray crystallography is the foremost method to acquire atomic resolution for macromolecules, the limiting step is obtaining protein crystals that can be useful of structure determination. High-throughput methods have been developed in recent years to clone, express, purify, crystallize and determine the three-dimensional structure of a protein gene product rapidly using automated devices, commercialized kits and consolidated protocols. However, the average number of protein structures obtained for most structural genomic groups has been very low compared to the total number of proteins purified. As more entire genomic sequences are obtained for different organisms from the three kingdoms of life, only the proteins that can be crystallized and whose structures can be obtained easily are studied. Consequently, an astonishing number of genomic proteins remain unexamined. In the era of high-throughput processes, traditional methods in molecular biology, protein chemistry and crystallization are eclipsed by automation and pipeline practices. The necessity for high-rate production of protein crystals and structures has prevented the usage of more intellectual strategies and creative approaches in experimental executions. Fundamental principles and personal experiences in protein chemistry and crystallization are minimally exploited only to obtain "low-hanging fruit" protein structures. We review the practical aspects of today's high-throughput manipulations and discuss the challenges in fast pace protein crystallization and tools for crystallography. Structural genomic pipelines can be improved with information gained from low-throughput tactics that may help us reach the higher-bearing fruits. Examples of recent developments in this area are reported from

  10. Life in the fast lane for protein crystallization and X-ray crystallography.

    Science.gov (United States)

    Pusey, Marc L; Liu, Zhi-Jie; Tempel, Wolfram; Praissman, Jeremy; Lin, Dawei; Wang, Bi-Cheng; Gavira, José A; Ng, Joseph D

    2005-07-01

    The common goal for structural genomic centers and consortiums is to decipher as quickly as possible the three-dimensional structures for a multitude of recombinant proteins derived from known genomic sequences. Since X-ray crystallography is the foremost method to acquire atomic resolution for macromolecules, the limiting step is obtaining protein crystals that can be useful of structure determination. High-throughput methods have been developed in recent years to clone, express, purify, crystallize and determine the three-dimensional structure of a protein gene product rapidly using automated devices, commercialized kits and consolidated protocols. However, the average number of protein structures obtained for most structural genomic groups has been very low compared to the total number of proteins purified. As more entire genomic sequences are obtained for different organisms from the three kingdoms of life, only the proteins that can be crystallized and whose structures can be obtained easily are studied. Consequently, an astonishing number of genomic proteins remain unexamined. In the era of high-throughput processes, traditional methods in molecular biology, protein chemistry and crystallization are eclipsed by automation and pipeline practices. The necessity for high-rate production of protein crystals and structures has prevented the usage of more intellectual strategies and creative approaches in experimental executions. Fundamental principles and personal experiences in protein chemistry and crystallization are minimally exploited only to obtain "low-hanging fruit" protein structures. We review the practical aspects of today's high-throughput manipulations and discuss the challenges in fast pace protein crystallization and tools for crystallography. Structural genomic pipelines can be improved with information gained from low-throughput tactics that may help us reach the higher-bearing fruits. Examples of recent developments in this area are reported from

  11. Development of an X-ray HARP–FEA detector system for high-throughput protein crystallography

    International Nuclear Information System (INIS)

    A new detector system for protein crystallography based on an X-ray HARP–FEA is presented. A new detector system for protein crystallography is now being developed based on an X-ray HARP–FEA (high-gain avalanche rushing amorphous photoconductor–field emitter array), which consists of an amorphous selenium membrane and a matrix field emitter array. The combination of the membrane avalanche effect with a single driven FEA has several advantages over currently available area detectors, including higher sensitivity, higher spatial resolution and a higher frame rate. Preliminary evaluation of the detector has been carried out and its effectiveness has been confirmed. Next, diffraction images were measured with continuous rotation of a protein crystal, and the images were compared with those measured by the existing CCD detector; the system successfully obtained high-spatial-resolution images. Using shutterless measurement, the total measurement time can be reduced significantly, making the method appropriate for high-throughput protein crystallography. The X-ray HARP–FEA detector is an attractive candidate for the next generation of X-ray area detectors

  12. Optimizing the spatial distribution of dose in X-ray macromolecular crystallography.

    Science.gov (United States)

    Zeldin, Oliver B; Gerstel, Markus; Garman, Elspeth F

    2013-01-01

    X-ray data collection for macromolecular crystallography can lead to highly inhomogeneous distributions of dose within the crystal volume for cases when the crystal is larger than the beam or when the beam is non-uniform (gaussian-like), particularly when crystal rotation is fully taken into account. Here the spatial distribution of dose is quantitatively modelled in order to compare the effectiveness of two dose-spreading data-collection protocols: helical scanning and translational collection. Their effectiveness in reducing the peak dose per unit diffraction is investigated via simulations for four common crystal shapes (cube, plate, long and short needles) and beams with a wide range of full width half maximum values. By inspection of the chosen metric, it is concluded that the optimum strategy is always to use as flat (top-hat) a beam as possible and to either match the beam size in both dimensions to the crystal, or to perform a helical scan with a beam which is narrow along the rotation axis and matched to the crystal size along the perpendicular axis. For crystal shapes where this is not possible, the reduction in peak dose per unit diffraction achieved through dose spreading is quantified and tabulated as a reference for experimenters.

  13. -2,4-Dichlorobenzoyl phosphoric triamides: Synthesis, spectroscopic and X-ray crystallography studies

    Indian Academy of Sciences (India)

    Khodayar Gholivand; Nasrin Oroujzadeh; Zahra Shariatinia

    2010-07-01

    New phosphoric triamides 1-9 were synthesized by the reaction of -2,4-dichlorobenzoyl phosphoramidic dichloride with various cyclic aliphatic amines and the products were characterized by 1H, 13C, 31P NMR, IR spectroscopy and elemental analysis. Surprisingly, the 1H NMR spectrum of 2 indicated long range 6 (P, H) coupling constant = 1.3, 1.4 Hz and those of molecules 3, 4, 6-8 display longrange 4 (H, H) coupling constants (1.8-1.9 Hz) for the coupling of aromatic protons in 2,4-dichlorophenyl rings. 1H NMR spectra indicated 3 (PNCH) for enantiotopic and diastereotopic benzylic CH2 protons in compounds 7 and 8. The spectroscopic data of newly synthesized compounds were compared with those related -benzoyl derivatives. The structures of compounds 5, 8 and 10 (2,4-Cl2-C6H3C(O)NHP(O)[NCH2CH(CH3)2]2) have been determined by X-ray crystallography. The structures form centrosymmetric dimers through intermolecular strong -P=O…H-N-hydrogen bonds. The dimers connect to each other via rather strong and weak C-H…O plus weak C-H…Cl H-bonds to produce a 1-D network for 5 while 3-D polymeric chains for 8 and 10.

  14. A split-beam probe-pump-probe scheme for femtosecond time resolved protein X-ray crystallography

    Directory of Open Access Journals (Sweden)

    Jasper J. van Thor

    2015-01-01

    Full Text Available In order to exploit the femtosecond pulse duration of X-ray Free-Electron Lasers (XFEL operating in the hard X-ray regime for ultrafast time-resolved protein crystallography experiments, critical parameters that determine the crystallographic signal-to-noise (I/σI must be addressed. For single-crystal studies under low absorbed dose conditions, it has been shown that the intrinsic pulse intensity stability as well as mode structure and jitter of this structure, significantly affect the crystallographic signal-to-noise. Here, geometrical parameters are theoretically explored for a three-beam scheme: X-ray probe, optical pump, X-ray probe (or “probe-pump-probe” which will allow experimental determination of the photo-induced structure factor amplitude differences, ΔF, in a ratiometric manner, thereby internally referencing the intensity noise of the XFEL source. In addition to a non-collinear split-beam geometry which separates un-pumped and pumped diffraction patterns on an area detector, applying an additional convergence angle to both beams by focusing leads to integration over mosaic blocks in the case of well-ordered stationary protein crystals. Ray-tracing X-ray diffraction simulations are performed for an example using photoactive yellow protein crystals in order to explore the geometrical design parameters which would be needed. The specifications for an X-ray split and delay instrument that implements both an offset angle and focused beams are discussed, for implementation of a probe-pump-probe scheme at the European XFEL. We discuss possible extension of single crystal studies to serial femtosecond crystallography, particularly in view of the expected X-ray damage and ablation due to the first probe pulse.

  15. Iterative Mass Spectrometry and X-Ray Crystallography to Study Ion-Trapping and Rearrangements by a Flexible Cluster

    OpenAIRE

    Zhang, Kun; Kurmoo, Mohamedally; Wei, Lian-Qiang; Zeng, Ming-Hua

    2013-01-01

    An important aspect of chemical reactions involves understanding the intermediate steps from reactants to products. The iterative use of mass spectrometry and X-Ray crystallography is demonstrated to be a powerful combination in this respect. We have applied them in identifying molecular clusters in solution followed by their solid-state structural characterizations. We used a key ligand, 2-[(2-hydroxy-3-methoxy-benzylidene)-amino]-ethanesulfonate (L), which serves as chelating/bridging units...

  16. Direct detection of x-rays for protein crystallography employing a thick, large area CCD

    Science.gov (United States)

    Atac, Muzaffer; McKay, Timothy

    1999-01-01

    An apparatus and method for directly determining the crystalline structure of a protein crystal. The crystal is irradiated by a finely collimated x-ray beam. The interaction of the x-ray beam with the crystal produces scattered x-rays. These scattered x-rays are detected by means of a large area, thick CCD which is capable of measuring a significant number of scattered x-rays which impact its surface. The CCD is capable of detecting the position of impact of the scattered x-ray on the surface of the CCD and the quantity of scattered x-rays which impact the same cell or pixel. This data is then processed in real-time and the processed data is outputted to produce a image of the structure of the crystal. If this crystal is a protein the molecular structure of the protein can be determined from the data received.

  17. NSLS-II Biomedical beamlines for macromolecular crystallography, FMX and AMX, and for X-ray scattering, LIX: current developments

    International Nuclear Information System (INIS)

    We present the current status of development of the two macromolecular crystallography (MX) beamlines, FMX and AMX, and the X-ray scattering beamline LIX, at the National Synchrotron Light Source-II (NSLS-II) [1]. Together, FMX and AMX will cover a broad range of use cases from serial crystallography on micron sized crystals, to very large unit cell complexes, to rapid sample screening, e.g. for the always-hard-to-grow membrane proteins and for ligand binding studies. The LIX beamline will support a variety of X-ray scattering measurements for studies on proteins in solution, lipid membranes and biological tissues. We have performed Synchrotron Radiation Workshop (SRW) [2] and Shadow[3] simulations to help select optimal methods to modify the size of the beam easily and smoothly at both FMX and AMX. The very low emittance of the NSLS-II storage ring and the resulting low divergence of the X-ray beam, as well as the long optical path lengths in the photon delivery systems lead to stringent requirements e.g. for vibrational stability and mirror quality. We discuss beamline design considerations addressing these challenges, such as combining mirror optics with compound refractive lenses (CRLs).

  18. An Excel Spreadsheet for a One-Dimensional Fourier Map in X-ray Crystallography

    Science.gov (United States)

    Clegg, William

    2004-01-01

    The teaching of crystal structure determination with single-crystal X-ray diffraction at undergraduate level faces numerous challenges. Single-crystal X-ray diffraction is used in a vast range of chemical research projects and forms the basis for a high proportion of structural results that are presented to high-school, undergraduate, and graduate…

  19. Ultrasonic acoustic levitation for fast frame rate X-ray protein crystallography at room temperature

    OpenAIRE

    Soichiro Tsujino; Takashi Tomizaki

    2016-01-01

    Increasing the data acquisition rate of X-ray diffraction images for macromolecular crystals at room temperature at synchrotrons has the potential to significantly accelerate both structural analysis of biomolecules and structure-based drug developments. Using lysozyme model crystals, we demonstrated the rapid acquisition of X-ray diffraction datasets by combining a high frame rate pixel array detector with ultrasonic acoustic levitation of protein crystals in liquid droplets. The rapid spinn...

  20. Crystallography using synchrotron radiation X-ray. Application of Weissenberg and time resolved Laue methods to macromolecular structure analysis

    International Nuclear Information System (INIS)

    The three-dimensional structures of macromolecules under static and dynamic conditions are very important for the study of molecular biology. X-ray crystallography is the most powerful tool to obtain the three-dimensional structures of the macromolecules of especially large size, for which synchrotron radiation X-ray is used, The collection of diffraction data is the first, most important step for crystalline structure analysis. Efforts have been exerted to establish the data collection system using monochromatic synchrotron radiation X-ray (SRX). The diffraction intensity data collection system combined with a newly developed Weissenberg camera for macromolecules and an image plate (IP) using SRX has been established at the Photon Factory. Many important biological structures by high resolution have already come out with this data collection system, which is used also for the study on enzymatic reaction mechanism. A time resolved Laue camera has been designed, and the preliminary experiment has been carried out in the Photon Factory. These systems are reported. (K.I.)

  1. CCD[charge-coupled device]-based synchrotron x-ray detector for protein crystallography: Performance projected from an experiment

    International Nuclear Information System (INIS)

    The intense x radiation from a synchrotron source could, with a suitable detector, provide a complete set of diffraction images from a protein crystal before the crystal is damaged by radiation (2 to 3 min). An area detector consisting of a 40 mm dia. x-ray fluorescing phosphor, coupled with an image intensifier and lens to a CCD image sensor, was developed to determine the effectiveness of such a detector in protein crystallography. The detector was used in an experiment with a rotating anode x-ray generator. Diffraction patterns from a lysozyme crystal obtained with this detector are compared to those obtained with film. The two images appear to be virtually identical. The flux of 104 x-ray photons/s was observed on the detector at the rotating anode generator. At the 6-GeV synchrotron being designed at Argonne, the flux on an 80 x 80 mm2 detector is expected to be >109 photons/s. The projected design of such a synchrotron detector shows that a diffraction-peak count >106 could be obtained in ∼0.5 s. With an additional ∼0.5 s readout time of a 512 x 512 pixel CCD, the data acquisition time per frame would be ∼1 s so that ninety 10 diffraction images could be obtained, with approximately 1% precision, in less than 3 min

  2. Crystallography using synchrotron radiation X-ray. Application of Weissenberg and time resolved Laue methods to macromolecular structure analysis

    Energy Technology Data Exchange (ETDEWEB)

    Sakabe, Noriyoshi [National Lab. for High Energy Physics, Tsukuba, Ibaraki (Japan)

    1994-12-31

    The three-dimensional structures of macromolecules under static and dynamic conditions are very important for the study of molecular biology. X-ray crystallography is the most powerful tool to obtain the three-dimensional structures of the macromolecules of especially large size, for which synchrotron radiation X-ray is used, The collection of diffraction data is the first, most important step for crystalline structure analysis. Efforts have been exerted to establish the data collection system using monochromatic synchrotron radiation X-ray (SRX). The diffraction intensity data collection system combined with a newly developed Weissenberg camera for macromolecules and an image plate (IP) using SRX has been established at the Photon Factory. Many important biological structures by high resolution have already come out with this data collection system, which is used also for the study on enzymatic reaction mechanism. A time resolved Laue camera has been designed, and the preliminary experiment has been carried out in the Photon Factory. These systems are reported. (K.I.).

  3. X-ray Damage to the Mn4Ca Complex in Single Crystals ofPhotosystem II: A Case Study for Metalloprotein Crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Kern, Jan; Irrgang, Klaus-Dieter; Latimer, Matthew; Bergmann, Uwe; Glatzel, Pieter; Pushkar, Yulia; Biesiadka, Jacek; Loll,Bernhard; Sauer, Kenneth; Messinger, Johannes; Zouni, Athina; Yachandra,Vittal K.

    2005-06-21

    X-ray absorption spectroscopy was used to measure the damage caused by exposure to X-rays to the Mn4Ca active site in single crystals of photosystem II, as a function of dose and energy of X-rays, temperature, and time. These studies reveal that the conditions used for structure determination by X-ray crystallography cause serious damage specifically to the metal-site structure. The X-ray absorption spectra show that the structure changes from one that is characteristic of a high-valent Mn4(III2,IV2) oxo-bridged Mn4Ca cluster, to that of Mn(II) in aqueous solution. This damage to the metal site occurs at a dose that is more than an order of magnitude lower than that resulting in loss of diffractivity, and commonly considered safe for protein crystallography. These results establish the first quantitative X-ray dose parameters applicable to redox-active metallo-proteins. This case study shows that a careful evaluation of the structural intactness of the active sites by spectroscopic techniques can validate structures derived from crystallography, and it can be a valuable complementary method before structure-function correlations of metallo-proteins can be made on the basis of high resolution X-ray crystal structures.

  4. X-ray damage to the Mn4Ca complex in single crystals of photosystem II: a case study for metalloprotein crystallography.

    Science.gov (United States)

    Yano, Junko; Kern, Jan; Irrgang, Klaus-Dieter; Latimer, Matthew J; Bergmann, Uwe; Glatzel, Pieter; Pushkar, Yulia; Biesiadka, Jacek; Loll, Bernhard; Sauer, Kenneth; Messinger, Johannes; Zouni, Athina; Yachandra, Vittal K

    2005-08-23

    X-ray absorption spectroscopy was used to measure the damage caused by exposure to x-rays to the Mn(4)Ca active site in single crystals of photosystem II as a function of dose and energy of x-rays, temperature, and time. These studies reveal that the conditions used for structure determination by x-ray crystallography cause serious damage specifically to the metal-site structure. The x-ray absorption spectra show that the structure changes from one that is characteristic of a high-valent Mn(4)(III(2),IV(2)) oxo-bridged Mn(4)Ca cluster to that of Mn(II) in aqueous solution. This damage to the metal site occurs at a dose that is more than one order of magnitude lower than the dose that results in loss of diffractivity and is commonly considered safe for protein crystallography. These results establish quantitative x-ray dose parameters that are applicable to redox-active metalloproteins. This case study shows that a careful evaluation of the structural intactness of the active site(s) by spectroscopic techniques can validate structures derived from crystallography and that it can be a valuable complementary method before structure-function correlations of metalloproteins can be made on the basis of high-resolution x-ray crystal structures.

  5. X-ray instrumentation for SR beamlines

    CERN Document Server

    Kovalchuk, M V; Zheludeva, S I; Aleshko-Ozhevsky, O P; Arutynyan, E H; Kheiker, D M; Kreines, A Y; Lider, V V; Pashaev, E M; Shilina, N Y; Shishkov, V A

    2000-01-01

    The main possibilities and parameters of experimental X-ray stations are presented: 'Protein crystallography', 'X-ray structure analysis', 'High-precision X-ray optics', 'X-ray crystallography and material science', 'X-ray topography', 'Photoelectron X-ray standing wave' that are being installed at Kurchatov SR source by A.V. Shubnikov Institute of Crystallography.

  6. X-ray Crystallography of A Metalloprotein: A Reaction Intermediate of Heme Oxygenase

    Science.gov (United States)

    Unno, Masaki; Matsui, Toshitaka; Ikeda-Saito, Masao

    X-ray crystallographic analysis of a metalloprotein requires knowing the electronic state of the metal center, if one wants to elucidate the exact function and/or reaction mechanism. As an example, we show our recent structural analysis of the heme oxygenase reaction intermediate which is involved in the third step of the heme degradation reaction. The reaction intermediate was crystallized under anaerobic condition, and the obtained crystals were frozen into liquid nitrogen. The absorption spectra of the single crystal before and after X-ray irradiation were compared with that of the frozen solution in 100 K cold nitrogen stream. The determined structure offers the first solid evidence for the presence of a water cluster in the distal pocket of this catalytically critical intermediate. This structure combined with the QM/MM calculation supports our proposal that the biliverdin is produced via Fe-OOH verdoheme intermediate.

  7. Hydrogen atoms can be located accurately and precisely by x-ray crystallography.

    Science.gov (United States)

    Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M; Woźniak, Krzysztof; Jayatilaka, Dylan

    2016-05-01

    Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A-H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A-H bond lengths with those from neutron measurements for A-H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors. PMID:27386545

  8. Hydrogen atoms can be located accurately and precisely by x-ray crystallography

    Science.gov (United States)

    Woińska, Magdalena; Grabowsky, Simon; Dominiak, Paulina M.; Woźniak, Krzysztof; Jayatilaka, Dylan

    2016-01-01

    Precise and accurate structural information on hydrogen atoms is crucial to the study of energies of interactions important for crystal engineering, materials science, medicine, and pharmacy, and to the estimation of physical and chemical properties in solids. However, hydrogen atoms only scatter x-radiation weakly, so x-rays have not been used routinely to locate them accurately. Textbooks and teaching classes still emphasize that hydrogen atoms cannot be located with x-rays close to heavy elements; instead, neutron diffraction is needed. We show that, contrary to widespread expectation, hydrogen atoms can be located very accurately using x-ray diffraction, yielding bond lengths involving hydrogen atoms (A–H) that are in agreement with results from neutron diffraction mostly within a single standard deviation. The precision of the determination is also comparable between x-ray and neutron diffraction results. This has been achieved at resolutions as low as 0.8 Å using Hirshfeld atom refinement (HAR). We have applied HAR to 81 crystal structures of organic molecules and compared the A–H bond lengths with those from neutron measurements for A–H bonds sorted into bonds of the same class. We further show in a selection of inorganic compounds that hydrogen atoms can be located in bridging positions and close to heavy transition metals accurately and precisely. We anticipate that, in the future, conventional x-radiation sources at in-house diffractometers can be used routinely for locating hydrogen atoms in small molecules accurately instead of large-scale facilities such as spallation sources or nuclear reactors.

  9. Radiation-damage-free quantum crystallography and resolution-enhanced x-ray imaging techniques using quantum multipath interference of thermal light

    CERN Document Server

    Li, Zheng; Medvedev, Nikita; Wang, Fenglin; Chapman, Henry N; Shih, Yanhua

    2016-01-01

    Using higher order coherence of thermal light sources, we can achieve enhancement of resolution of standard x-ray imaging techniques, such as x-ray diffraction and phase contrast imaging. The cost of implementing such schemes is minimal comparing to the schemes using entangled two-photon pairs. The proposed diffractive quan- tum crystallography using multipath interference of thermal light can be eventually free of radiation damage, because the diffraction pattern could be formed by using low energy photons of optical wavelength. Thus it is promising to apply the proposed quantum crystallography scheme to nanocrystalline or non-crystalline samples that are too difficult to be crystallized.

  10. Synthesis and structure elucidation of a series of pyranochromene chalcones and flavanones using 1D and 2D NMR spectroscopy and X-ray crystallography.

    Science.gov (United States)

    Pawar, Sunayna S; Koorbanally, Neil A

    2014-06-01

    A series of novel pyranochromene chalcones and corresponding flavanones were synthesized. This is the first report on the confirmation of the absolute configuration of chromene-based flavanones using X-ray crystallography. These compounds were characterized by 2D NMR spectroscopy, and their assignments are reported herein. The 3D structure of the chalcone 3b and flavanone 4g was determined by X-ray crystallography, and the structure of the flavanone was confirmed to be in the S configuration at C-2.

  11. FIST - a suite of X-ray powder crystallography programs for use with a HP-65 calculator

    International Nuclear Information System (INIS)

    Programs for X-ray powder crystallography are defined for use with a Hewlett Packard HP-65 (programmable) pocket calculator. These include the prediction of all Bragg reflections for defined P-, F-, I-cubic, tetragonal, hexagonal and orthorhombic cells; the calculation of the position of a specific Bragg reflection from defined unit cells with all symmetries except triclinic; interconversion of theta, 2theta, sin2theta and d, as well as the calculation of the Nelson-Riley function; the computation of crystal densities; the interconversion of rhombohedral and hexagonal unit cells, lsub(c) determinations for graphite, the calculation of a and c for boron carbide; and Miller index transformations between various unit cells. (author)

  12. Analysis of cytochrome P450 CYP119 ligand-dependent conformational dynamics by two-dimensional NMR and X-ray crystallography.

    Science.gov (United States)

    Basudhar, Debashree; Madrona, Yarrow; Kandel, Sylvie; Lampe, Jed N; Nishida, Clinton R; de Montellano, Paul R Ortiz

    2015-04-17

    Defining the conformational states of cytochrome P450 active sites is critical for the design of agents that minimize drug-drug interactions, the development of isoform-specific P450 inhibitors, and the engineering of novel oxidative catalysts. We used two-dimensional (1)H,(15)N HSQC chemical shift perturbation mapping of (15)N-labeled Phe residues and x-ray crystallography to examine the ligand-dependent conformational dynamics of CYP119. Active site Phe residues were most affected by the binding of azole inhibitors and fatty acid substrates, in agreement with active site localization of the conformational changes. This was supported by crystallography, which revealed movement of the F-G loop with various azoles. Nevertheless, the NMR chemical shift perturbations caused by azoles and substrates were distinguishable. The absence of significant chemical shift perturbations with several azoles revealed binding of ligands to an open conformation similar to that of the ligand-free state. In contrast, 4-phenylimidazole caused pronounced NMR changes involving Phe-87, Phe-144, and Phe-153 that support the closed conformation found in the crystal structure. The same closed conformation is observed by NMR and crystallography with a para-fluoro substituent on the 4-phenylimidazole, but a para-chloro or bromo substituent engendered a second closed conformation. An open conformation is thus favored in solution with many azole ligands, but para-substituted phenylimidazoles give rise to two closed conformations that depend on the size of the para-substituent. The results suggest that ligands selectively stabilize discrete cytochrome P450 conformational states.

  13. Kissing G domains of MnmE monitored by X-ray crystallography and pulse electron paramagnetic resonance spectroscopy.

    Directory of Open Access Journals (Sweden)

    Simon Meyer

    2009-10-01

    Full Text Available MnmE, which is involved in the modification of the wobble position of certain tRNAs, belongs to the expanding class of G proteins activated by nucleotide-dependent dimerization (GADs. Previous models suggested the protein to be a multidomain protein whose G domains contact each other in a nucleotide dependent manner. Here we employ a combined approach of X-ray crystallography and pulse electron paramagnetic resonance (EPR spectroscopy to show that large domain movements are coupled to the G protein cycle of MnmE. The X-ray structures show MnmE to be a constitutive homodimer where the highly mobile G domains face each other in various orientations but are not in close contact as suggested by the GDP-AlF(x structure of the isolated domains. Distance measurements by pulse double electron-electron resonance (DEER spectroscopy show that the G domains adopt an open conformation in the nucleotide free/GDP-bound and an open/closed two-state equilibrium in the GTP-bound state, with maximal distance variations of 18 A. With GDP and AlF(x, which mimic the transition state of the phosphoryl transfer reaction, only the closed conformation is observed. Dimerization of the active sites with GDP-AlF(x requires the presence of specific monovalent cations, thus reflecting the requirements for the GTPase reaction of MnmE. Our results directly demonstrate the nature of the conformational changes MnmE was previously suggested to undergo during its GTPase cycle. They show the nucleotide-dependent dynamic movements of the G domains around two swivel positions relative to the rest of the protein, and they are of crucial importance for understanding the mechanistic principles of this GAD.

  14. Structural Elucidation of Dendritic Host-Guest Complexes by X-ray Crystallography and Molecular Dynamics Simulations

    OpenAIRE

    Chang, T; Pieterse, K.; Broeren, M.A.C.; Kooijman, H.; Spek, A.L.; Hilbers, M.F.; Meijer, E. W.

    2007-01-01

    The multiple monovalent binding of adamantyl-urea poly(propyleneimine) dendrimers with carboxylic acid-urea guests was investigated using molecular dynamics simulations and Xray crystallography to better understand the structure and behavior of the dynamic multivalent complex in solution. The results from the two methods are consistent and suggest a preferred molecular picture of this complicated aggregate of multiple components. The guest molecules can bind to the dendrimer in a variety of w...

  15. Metalloprotein structures at ambient conditions and in real-time: biological crystallography and spectroscopy using X-ray free electron lasers.

    Science.gov (United States)

    Kern, Jan; Yachandra, Vittal K; Yano, Junko

    2015-10-01

    Although the structure of enzymes and the chemistry at the catalytic sites have been studied intensively, an understanding of the atomic-scale chemistry requires a new approach beyond steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure of metallo-enzymes at ambient conditions, while overcoming the severe X-ray-induced changes to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by the intense and ultra-short femtosecond (fs) X-ray pulses from an X-ray free electron laser (XFEL) by acquiring a signal before the sample is destroyed. This review describes the recent and pioneering uses of XFELs to study the protein structure and dynamics of metallo-enzymes using crystallography and scattering, as well as the chemical structure and dynamics of the catalytic complexes (charge, spin, and covalency) using spectroscopy during the reaction to understand the electron-transfer processes and elucidate the mechanism.

  16. Inhibition of d-xylose isomerase by polyols: atomic details by joint X-ray/neutron crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Kovalevsky, Andrey, E-mail: ayk@lanl.gov [Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States); Hanson, B. Leif [University of Toledo, 2801 West Bancroft Street, Toledo, OH 43606 (United States); Mason, Sax A. [Institut Laue–Langevin, 6 Rue Jules Horowitz, 38042 Grenoble (France); Forsyth, V. Trevor [Institut Laue–Langevin, 6 Rue Jules Horowitz, 38042 Grenoble (France); Keele University, Staffordshire (United Kingdom); Fisher, Zoe [Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States); Mustyakimov, Marat [Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States); Oak Ridge National Laboratory, PO Box 2008, MS 6475, Oak Ridge, TN 37831 (United States); Blakeley, Matthew P. [Institut Laue–Langevin, 6 Rue Jules Horowitz, 38042 Grenoble (France); Keen, David A. [Harwell Science and Innovation Campus, Didcot, Oxon OX11 0QX (United Kingdom); Langan, Paul [Oak Ridge National Laboratory, PO Box 2008, MS 6475, Oak Ridge, TN 37831 (United States); Los Alamos National Laboratory, PO Box 1663, MS M888, Los Alamos, NM 87545 (United States)

    2012-09-01

    A joint X-ray/neutron structure of d-xylose isomerase in complex with the inhibitor sorbitol was determined at room temperature at an acidic pH of 5.9. Protonation of the O5 O atom of the sugar was directly observed in the nuclear density maps. Under acidic conditions sorbitol gains a water-mediated interaction with the enzyme active site, which may explain the increased potency of the inhibitor at low pH. d-Xylose isomerase (XI) converts the aldo-sugars xylose and glucose to their keto analogs xylulose and fructose, but is strongly inhibited by the polyols xylitol and sorbitol, especially at acidic pH. In order to understand the atomic details of polyol binding to the XI active site, a 2.0 Å resolution room-temperature joint X-ray/neutron structure of XI in complex with Ni{sup 2+} cofactors and sorbitol inhibitor at pH 5.9 and a room-temperature X-ray structure of XI containing Mg{sup 2+} ions and xylitol at the physiological pH of 7.7 were obtained. The protonation of oxygen O5 of the inhibitor, which was found to be deprotonated and negatively charged in previous structures of XI complexed with linear glucose and xylulose, was directly observed. The Ni{sup 2+} ions occupying the catalytic metal site (M2) were found at two locations, while Mg{sup 2+} in M2 is very mobile and has a high B factor. Under acidic conditions sorbitol gains a water-mediated interaction that connects its O1 hydroxyl to Asp257. This contact is not found in structures at basic pH. The new interaction that is formed may improve the binding of the inhibitor, providing an explanation for the increased affinity of the polyols for XI at low pH.

  17. Inhibition of d-xylose isomerase by polyols: atomic details by joint X-ray/neutron crystallography

    International Nuclear Information System (INIS)

    A joint X-ray/neutron structure of d-xylose isomerase in complex with the inhibitor sorbitol was determined at room temperature at an acidic pH of 5.9. Protonation of the O5 O atom of the sugar was directly observed in the nuclear density maps. Under acidic conditions sorbitol gains a water-mediated interaction with the enzyme active site, which may explain the increased potency of the inhibitor at low pH. d-Xylose isomerase (XI) converts the aldo-sugars xylose and glucose to their keto analogs xylulose and fructose, but is strongly inhibited by the polyols xylitol and sorbitol, especially at acidic pH. In order to understand the atomic details of polyol binding to the XI active site, a 2.0 Å resolution room-temperature joint X-ray/neutron structure of XI in complex with Ni2+ cofactors and sorbitol inhibitor at pH 5.9 and a room-temperature X-ray structure of XI containing Mg2+ ions and xylitol at the physiological pH of 7.7 were obtained. The protonation of oxygen O5 of the inhibitor, which was found to be deprotonated and negatively charged in previous structures of XI complexed with linear glucose and xylulose, was directly observed. The Ni2+ ions occupying the catalytic metal site (M2) were found at two locations, while Mg2+ in M2 is very mobile and has a high B factor. Under acidic conditions sorbitol gains a water-mediated interaction that connects its O1 hydroxyl to Asp257. This contact is not found in structures at basic pH. The new interaction that is formed may improve the binding of the inhibitor, providing an explanation for the increased affinity of the polyols for XI at low pH

  18. Iterative mass spectrometry and X-ray crystallography to study ion-trapping and rearrangements by a flexible cluster.

    Science.gov (United States)

    Zhang, Kun; Kurmoo, Mohamedally; Wei, Lian-Qiang; Zeng, Ming-Hua

    2013-01-01

    An important aspect of chemical reactions involves understanding the intermediate steps from reactants to products. The iterative use of mass spectrometry and X-Ray crystallography is demonstrated to be a powerful combination in this respect. We have applied them in identifying molecular clusters in solution followed by their solid-state structural characterizations. We used a key ligand, 2-[(2-hydroxy-3-methoxy-benzylidene)-amino]-ethanesulfonate (L), which serves as chelating/bridging units to stabilize the precursor [Li₄Ni₆(OH)₂(L)₆(CH₃CN)₆](ClO₄)₂·4CH₃CN. The results of subsequent reactions witness a cascade of processes involving fragmentation, inner bridging ligand substitution (OH⁻ to OCH₃⁻), changing modes of binding (chelate to monodentate) of the key ligand, ion-trapping and exchange (Li⁺, Na⁺ and Ca²⁺) and their site preferences, coordinating and non-coordinating solvents (CH₃CN to CH₃OH, H₂O and EtOH) replacement. The flexibility of the Ni₃OL₃ species in solution permits the formation of six derivatives. The complimentary techniques open a broader prospect for cluster design and applications. PMID:24343303

  19. C-shaped diastereomers containing cofacial thiophene-substituted quinoxaline rings: synthesis, photophysical properties, and X-ray crystallography.

    Science.gov (United States)

    DeBlase, Catherine R; Finke, Ryan T; Porras, Jonathan A; Tanski, Joseph M; Nadeau, Jocelyn M

    2014-05-16

    Synthesis and characterization of two diastereomeric C-shaped molecules containing cofacial thiophene-substituted quinoxaline rings are described. A previously known bis-α-diketone was condensed with an excess of 4-bromo-1,2-diaminobenzene in the presence of zinc acetate to give a mixture of two C-shaped diastereomers with cofacial bromine-substituted quinoxaline rings. After chromatographic separation, thiophene rings were installed by a microwave-assisted Suzuki coupling reaction, resulting in highly emissive diastereomeric compounds that were studied by UV-vis, fluorescence, and NMR spectroscopy, as well as X-ray crystallography. The unique symmetry of each diastereomer was confirmed by NMR spectroscopy. NMR data indicated that the syn isomer has restricted rotation about the bond connecting the thiophene and quinoxaline rings, which was also observed in the solid state. The spectroscopic properties of the C-shaped diastereomers were compared to a model compound containing only a single thiophene-substituted quinoxaline ring. Ground state intramolecular π-π interactions in solution were detected by NMR and UV-vis spectroscopy. Red-shifted emission bands, band broadening, and large Stokes shifts were observed, which collectively suggest excited state π-π interactions that produce excimer-like emissions, as well as a remarkable positive emission solvatochromism, indicating charge-transfer character in the excited state.

  20. Structural Properties of Human CaMKII Ca2+ /Calmodulin-Dependent Protein Kinase II using X-ray Crystallography

    Science.gov (United States)

    Cao, Yumeng Melody; McSpadden, Ethan; Kuriyan, John; Department of Molecular; Cell Biology; Department of Chemistry Team

    To this day, human memory storage remains a mystery as we can at most describe the process vaguely on a cellular level. Switch-like properties of Calcium/Calmodulin-Dependent Protein Kinase II make it a leading candidate in understanding the molecular basis of human memory. The protein crystal was placed in the beam of a synchrotron source and the x-ray crystallography data was collected as reflections on a diffraction pattern that undergo Fourier transform to obtain the electron density. We observed two drastic differences from our solved structure at 2.75Å to a similar construct of the mouse CaMKII association domain. Firstly, our structure is a 6-fold symmetric dodecamer, whereas the previously published construct was a 7-fold symmetric tetradecamer. This suggests the association domain of human CaMKII is a dynamic structure that is triggered subunit exchange process. Secondly, in our structure the N-terminal tag is docked as an additional beta-strand on an uncapped beta-sheet present in each association domain protomer. This is concrete evidence of the involvement of the polypeptide docking site in the molecular mechanism underlining subunit exchange. In the future, we would like to selectively inhibit the exchange process while not disrupting the other functionalities of CaMKII.

  1. High-throughput plasmid construction using homologous recombination in yeast: its mechanisms and application to protein production for X-ray crystallography.

    Science.gov (United States)

    Mizutani, Kimihiko

    2015-01-01

    Homologous recombination is a system for repairing the broken genomes of living organisms by connecting two DNA strands at their homologous sequences. Today, homologous recombination in yeast is used for plasmid construction as a substitute for traditional methods using restriction enzymes and ligases. This method has various advantages over the traditional method, including flexibility in the position of DNA insertion and ease of manipulation. Recently, the author of this review reported the construction of plasmids by homologous recombination in the methanol-utilizing yeast Pichia pastoris, which is known to be an excellent expression host for secretory proteins and membrane proteins. The method enabled high-throughput construction of expression systems of proteins using P. pastoris; the constructed expression systems were used to investigate the expression conditions of membrane proteins and to perform X-ray crystallography of secretory proteins. This review discusses the mechanisms and applications of homologous recombination, including the production of proteins for X-ray crystallography.

  2. Mapping the topographic epitope landscape on the urokinase plasminogen activator receptor (uPAR) by surface plasmon resonance and X-ray crystallography

    DEFF Research Database (Denmark)

    Zhao, Baoyu; Gandhi, Sonu; Yuan, Cai;

    2015-01-01

    The urokinase-type plasminogen activator receptor (uPAR or CD87) is a glycolipid-anchored membrane protein often expressed in the microenvironment of invasive solid cancers and high levels are generally associated with poor patient prognosis (Kriegbaum et al., 2011 [1]). uPAR is organized as a dy...... of these mAbs by X-ray crystallography alone and in complex with uPAR [deposited in the PDB database as 4QTH and 4QTI, respectively]....

  3. Probing the Role of Divalent Metal Ions in a Bacterial Psychrophilic Metalloprotease: Binding Studies of an Enzyme in the Crystalline State by X-Ray Crystallography

    OpenAIRE

    Ravaud, Stephanie; Gouet, Patrice; Haser, Richard; Aghajari, Nushin

    2003-01-01

    The psychrophilic alkaline metalloprotease (PAP) produced by a Pseudomonas bacterium isolated in Antarctica belongs to the clan of metzincins, for which a zinc ion is essential for catalytic activity. Binding studies in the crystalline state have been performed by X-ray crystallography in order to improve the understanding of the role of the zinc and calcium ions bound to this protease. Cocrystallization and soaking experiments with EDTA in a concentration range from 1 to 85 mM have resulted ...

  4. On-line optical and X-ray spectroscopies with crystallography: an integrated approach for determining metalloprotein structures in functionally well defined states.

    Science.gov (United States)

    Ellis, Mark J; Buffey, Steven G; Hough, Michael A; Hasnain, S Samar

    2008-09-01

    X-ray-induced redox changes can lead to incorrect assignments of the functional states of metals in metalloprotein crystals. The need for on-line monitoring of the status of metal ions (and other chromophores) during protein crystallography experiments is of growing importance with the use of intense synchrotron X-ray beams. Significant efforts are therefore being made worldwide to combine different spectroscopies in parallel with X-ray crystallographic data collection. Here the implementation and utilization of optical and X-ray absorption spectroscopies on the modern macromolecular crystallography (MX) beamline 10, at the SRS, Daresbury Laboratory, is described. This beamline is equipped with a dedicated monolithic energy-dispersive X-ray fluorescence detector, allowing X-ray absorption spectroscopy (XAS) measurements to be made in situ on the same crystal used to record the diffraction data. In addition, an optical microspectrophotometer has been incorporated on the beamline, thus facilitating combined MX, XAS and optical spectroscopic measurements. By uniting these techniques it is also possible to monitor the status of optically active and optically silent metal centres present in a crystal at the same time. This unique capability has been applied to observe the results of crystallographic data collection on crystals of nitrite reductase from Alcaligenes xylosoxidans, which contains both type-1 and type-2 Cu centres. It is found that the type-1 Cu centre photoreduces quickly, resulting in the loss of the 595 nm peak in the optical spectrum, while the type-2 Cu centre remains in the oxidized state over a much longer time period, for which independent confirmation is provided by XAS data as this centre has an optical spectrum which is barely detectable using microspectrophotometry. This example clearly demonstrates the importance of using two on-line methods, spectroscopy and XAS, for identifying well defined redox states of metalloproteins during

  5. X-ray crystal structure of N-6 adenine deoxyribose nucleic acid methyltransferase from Streptococcus pneumoniae

    Science.gov (United States)

    Tran, Phidung Hong

    X-ray diffraction by using resonant anomalous scattering has become a popular tool for solving crystal structures in the last ten years with the expanded availability of tunable synchrotron radiation for protein crystallography. Mercury atoms were used for phasing. The crystal structure of N-6 deoxyribose nucleic acid methyltransferase from Streptoccocus pneumoniae (DpnM) was solved by using the Multiple Anomalous Diffraction technique. The crystal structure reveals the formation of mercaptide between the mercury ion and the thiol group on the cysteine amino acid in a hydrophobic environment. The crystal structure contains the bound ligand, S- adenosyl-l-methionine on the surface of the concave opening. The direction of the β-strands on the beta sheets are identical to other solved methyltransferases. The highly conserved motifs, DPPY and the FxGxG, are found to be important in ligand binding and possibly in methyl group transfer. The structure has a concave cleft with an opening on the order of 30 Å that can accommodate a DNA duplex. By molecular modelling coupled to sequence alignment, two other highly conserved residues Arg21 and Gly19 are found to be important in catalysis.

  6. Room-temperature serial crystallography using a kinetically optimized microfluidic device for protein crystallization and on-chip X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Michael Heymann

    2014-09-01

    Full Text Available An emulsion-based serial crystallographic technology has been developed, in which nanolitre-sized droplets of protein solution are encapsulated in oil and stabilized by surfactant. Once the first crystal in a drop is nucleated, the small volume generates a negative feedback mechanism that lowers the supersaturation. This mechanism is exploited to produce one crystal per drop. Diffraction data are measured, one crystal at a time, from a series of room-temperature crystals stored on an X-ray semi-transparent microfluidic chip, and a 93% complete data set is obtained by merging single diffraction frames taken from different unoriented crystals. As proof of concept, the structure of glucose isomerase was solved to 2.1 Å, demonstrating the feasibility of high-throughput serial X-ray crystallography using synchrotron radiation.

  7. The electron density of a-Oxalic acid dihydrate at 100 K by X-ray diffraction: a contribution to the IUCr Commission on Charge, Spin and Momentum Densities project on the accurate determination of electron densities

    NARCIS (Netherlands)

    Dam, J.; Harkema, S.; Feil, D.

    1983-01-01

    The results of the determination of the electron density of u-oxalic acid dihydrate at 100 K by means of X-ray diffraction are reported as part of the project on the accurate determination of electron densities which was initiated by the International Union of Crystallography. An extensive data set,

  8. Clear as Crystal: The Story of the Braggs--How X-Ray Crystallography Has Contributed to Science

    Science.gov (United States)

    George, Robert; Patterson, John

    2014-01-01

    Here is a brief history of the work of two of Australia's most famous scientists, Sir William Bragg and his son Sir Lawrence Bragg. Jointly awarded the Nobel Prize in 1915 for their groundbreaking research into the use of X-rays to study the chemical structure and function of molecules, they have contributed to our heritage and to science at…

  9. Chromium(III) Complex Obtained from Dipicolinic Acid: Synthesis, Characterization, X-Ray Crystal Structure and Electrochemical Studies

    Energy Technology Data Exchange (ETDEWEB)

    Ghasemi, Khaled; Rezvani, Ali Reza; Ghasemi, Fatemeh [Univ. of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of); Razak, Ibrahim Abdul; Rosli, Mohd Mustaqim [Universiti Sains Malaysia, Penang (Malaysia)

    2013-10-15

    The synthesis, X-ray crystallography, spectroscopic (IR, UV-vis), and electrochemical properties of the title compound, [H{sub 3}O][Cr(dipic){sub 2}] [H{sub 3}O{sup +}.Cl{sup -}] (1), (H{sub 2}dipic = 2,6-pyridinedicarboxylic acid), are reported. This complex crystallizes in the monoclinic space group Cc with a = 14.9006(10) A, b = 12.2114(8) A, c = 8.6337(6) A, α = 90.00 .deg., β = 92.7460(10) .deg., γ = 90.00 .deg., and V = 1569.16(18) A3 with Z = 4. The hydrogen bonding and noncovalent interactions play roles in the stabilization of the structure. In order to gain a better understanding of the most important geometrical parameters in the structure of the complex, atoms in molecules (AIM) method at B3LYP/6-31G level of theory has been employed.

  10. Determination of plutonium in nitric acid solutions using energy dispersive L X-ray fluorescence with a low power X-ray generator

    Energy Technology Data Exchange (ETDEWEB)

    Py, J. [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France); Groetz, J.-E., E-mail: jegroetz@univ-fcomte.fr [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Hubinois, J.-C.; Cardona, D. [Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France)

    2015-04-21

    This work presents the development of an in-line energy dispersive L X-ray fluorescence spectrometer set-up, with a low power X-ray generator and a secondary target, for the determination of plutonium concentration in nitric acid solutions. The intensity of the L X-rays from the internal conversion and gamma rays emitted by the daughter nuclei from plutonium is minimized and corrected, in order to eliminate the interferences with the L X-ray fluorescence spectrum. The matrix effects are then corrected by the Compton peak method. A calibration plot for plutonium solutions within the range 0.1–20 g L{sup −1} is given.

  11. Isolation and Characterization, Including by X-ray Crystallography, of Contact and Solvent-Separated Ion Pairs of Silenyl Lithium Species.

    Science.gov (United States)

    Pinchuk, Daniel; Mathew, Jomon; Kaushansky, Alexander; Bravo-Zhivotovskii, Dmitry; Apeloig, Yitzhak

    2016-08-22

    Reaction of bromoacylsilane 1 (pink solution) with tBu2 MeSiLi (3.5 equiv) in a 4:1 hexane:THF solvent mixture at -78 °C to room temperature yields the solvent separated ion pair (SSIP) of silenyl lithium E-[(tBuMe2 Si)(tBu2 MeSi)C=Si(SiMetBu2 )](-) [Li⋅4THF](+) 2 a (green-blue solution). Removal of the solvent and addition of benzene converts 2 a into the corresponding contact ion pair (CIP) 2 b (violet-red solution) with two THF molecules bonded to the lithium atom. The 2 a⇌2 b interconversion is reversible upon THF⇌ benzene solvent change. Both 2 a and 2 b were characterized by X-ray crystallography, NMR and UV/Vis spectroscopy, and theoretical calculations. The degree of dissociation of the Si-Li bond has a large effect on the visible spectrum (and thus color) and on the silenylic (29) Si NMR chemical shift, but a small effect on the molecular structure. This is the first report of the X-ray molecular structure of both the SSIP and the CIP of any R2 E=E'RM species (E=C, Si; E'=C, Si; M=metal). PMID:27466152

  12. Toward resolving the catalytic mechanism of dihydrofolate reductase using neutron and ultrahigh-resolution X-ray crystallography [Neutron and ultrahigh resolution X-ray crystallography reveals water as the proton donor in the catalytic mechanism of dihydrofolate reductase

    International Nuclear Information System (INIS)

    Dihydrofolate reductase (DHFR) catalyzes the NADPH-dependent reduction of dihydrofolate (DHF) to tetrahydrofolate (THF). An important step in the mechanism involves proton donation to the N5 atom of DHF. The inability to determine the protonation states of active site residues and substrate has led to the lack of consensus on a catalytic mechanism. To resolve this ambiguity, we conducted neutron and ultrahigh resolution X-ray crystallographic studies of the pseudo-Michaelis ternary complex of DHFR with folate and NADP+ from E. coli. The neutron data were collected to 2.0 Å resolution using a 3.6 mm3 crystal with the quasi-Laue technique, and the structure reveals that the N3 atom of folate is protonated while Asp27 is negatively charged. Previous mechanisms have proposed a keto-to-enol tautomerization of the substrate to facilitate protonation of the N5 atom. The structure supports the existence of the keto tautomer due to protonation of the N3 atom, suggesting tautomerization is unnecessary for catalysis. In the 1.05 Å resolution X-ray structure of the ternary complex, conformational disorder of the Met20 side chain is coupled to electron density for a partially occupied water within hydrogen-bonding distance of the N5 atom of folate; this suggests direct protonation of substrate by solvent. We propose a catalytic mechanism for DHFR that involves stabilization of the keto tautomer of the substrate, elevation of the pKa of the N5 atom of DHF by Asp27, and protonation of N5 by water whose access to the active site is gated by fluctuation of the Met20 side chain even though the Met-20 loop is closed

  13. Low-Z polymer sample supports for fixed-target serial femtosecond X-ray crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Feld, Geoffrey K. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); National Institute of Environmental Health Science, Research Triangle Park, NC (United States); Heymann, Michael [Brandeis Univ., Waltham, MA (United States); Univ. of Hamburg and DESY, Hamburg (Germany); Benner, W. Henry [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Pardini, Tommaso [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Tsai, Ching -Ju [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Boutet, Sebastien [SLAC National Accelerator Lab., Menlo Park, CA (United States); Coleman, Matthew A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Hunter, Mark S. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); SLAC National Accelerator Lab., Menlo Park, CA (United States); Li, Xiaodan [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Messerschmidt, Marc [SLAC National Accelerator Lab., Menlo Park, CA (United States); BioXFEL Science and Technology Center, Buffalo, NY (United States); Opathalage, Achini [Brandeis Univ., Waltham, MA (United States); Pedrini, Bill [Paul Scherrer Inst. (PSI), Villigen (Switzerland); Williams, Garth J. [SLAC National Accelerator Lab., Menlo Park, CA (United States); Krantz, Bryan A. [Univ. of California, Berkeley, CA (United States); Fraden, Seth [Brandeis Univ., Waltham, MA (United States); Hau-Riege, Stefan [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Evans, James E. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Segelke, Brent W. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Frank, Matthias [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2015-06-27

    X-ray free-electron lasers (XFELs) offer a new avenue to the structural probing of complex materials, including biomolecules. Delivery of precious sample to the XFEL beam is a key consideration, as the sample of interest must be serially replaced after each destructive pulse. The fixed-target approach to sample delivery involves depositing samples on a thin-film support and subsequent serial introduction via a translating stage. Some classes of biological materials, including two-dimensional protein crystals, must be introduced on fixed-target supports, as they require a flat surface to prevent sample wrinkling. A series of wafer and transmission electron microscopy (TEM)-style grid supports constructed of low-Z plastic have been custom-designed and produced. Aluminium TEM grid holders were engineered, capable of delivering up to 20 different conventional or plastic TEM grids using fixed-target stages available at the Linac Coherent Light Source (LCLS). As proof-of-principle, X-ray diffraction has been demonstrated from two-dimensional crystals of bacteriorhodopsin and three-dimensional crystals of anthrax toxin protective antigen mounted on these supports at the LCLS. In conclusion, the benefits and limitations of these low-Z fixed-target supports are discussed; it is the authors' belief that they represent a viable and efficient alternative to previously reported fixed-target supports for conducting diffraction studies with XFELs.

  14. Room-temperature serial crystallography at synchrotron X-ray sources using slowly flowing free-standing high-viscosity microstreams.

    Science.gov (United States)

    Botha, Sabine; Nass, Karol; Barends, Thomas R M; Kabsch, Wolfgang; Latz, Beatrice; Dworkowski, Florian; Foucar, Lutz; Panepucci, Ezequiel; Wang, Meitian; Shoeman, Robert L; Schlichting, Ilme; Doak, R Bruce

    2015-02-01

    Recent advances in synchrotron sources, beamline optics and detectors are driving a renaissance in room-temperature data collection. The underlying impetus is the recognition that conformational differences are observed in functionally important regions of structures determined using crystals kept at ambient as opposed to cryogenic temperature during data collection. In addition, room-temperature measurements enable time-resolved studies and eliminate the need to find suitable cryoprotectants. Since radiation damage limits the high-resolution data that can be obtained from a single crystal, especially at room temperature, data are typically collected in a serial fashion using a number of crystals to spread the total dose over the entire ensemble. Several approaches have been developed over the years to efficiently exchange crystals for room-temperature data collection. These include in situ collection in trays, chips and capillary mounts. Here, the use of a slowly flowing microscopic stream for crystal delivery is demonstrated, resulting in extremely high-throughput delivery of crystals into the X-ray beam. This free-stream technology, which was originally developed for serial femtosecond crystallography at X-ray free-electron lasers, is here adapted to serial crystallography at synchrotrons. By embedding the crystals in a high-viscosity carrier stream, high-resolution room-temperature studies can be conducted at atmospheric pressure using the unattenuated X-ray beam, thus permitting the analysis of small or weakly scattering crystals. The high-viscosity extrusion injector is described, as is its use to collect high-resolution serial data from native and heavy-atom-derivatized lysozyme crystals at the Swiss Light Source using less than half a milligram of protein crystals. The room-temperature serial data allow de novo structure determination. The crystal size used in this proof-of-principle experiment was dictated by the available flux density. However, upcoming

  15. Insight Into the Radical Mechanism of Phycocyanobilin-Ferredoxin Oxidoreductase (Pcya) Revealed By X-Ray Crystallography And Biochemical Measurements

    Energy Technology Data Exchange (ETDEWEB)

    Tu, S.-L.; Rockwell, N.; Lagarias, J.C.; Fisher, A.J.; /Inst. Plant Microb. Biol., Taipei /UC, Davis

    2007-07-13

    The X-ray crystal structure of the substrate-free form of phycocyanobilin (PCB)-ferredoxin oxidoreductase (PcyA; EC 1.3.7.5) from the cyanobacterium Nostoc sp. PCC7120 has been solved at 2.5 angstrom resolution. A comparative analysis of this structure with those recently reported for substrate-bound and substrate-free forms of PcyA from the cyanobacterium Synechocystis sp. PCC6803 (Hagiwara et al. (2006) Proc. Natl. Acad. Sci. U.S.A. 103, 27-32; Hagiwara et al. (2006) FEBS Lett. 580, 3823-3828) provides a compelling picture of substrate-induced changes in the PcyA enzyme and the chemical basis of PcyA's catalytic activity. On the basis of these structures and the biochemical analysis of site-directed mutants of Nostoc PcyA, including mutants reported in recent studies (Tu et al. (2006) J. Biol. Chem. 281, 3127-3136) as well as mutants described in this study, a revised mechanism for the PcyA-mediated four-electron reduction of biliverdin IX{alpha} to 3E/3Z-phycocyanobilin via enzyme-bound bilin radical intermediates is proposed. The mechanistic insight of these studies, along with homology modeling, have provided new insight into the catalytic mechanisms of other members of the ferredoxin-dependent bilin reductase family that are widespread in oxygenic photosynthetic organisms.

  16. New insight into the dynamic properties and the active site architecture of H-Ras p21 revealed by X-ray crystallography at very high resolution

    Directory of Open Access Journals (Sweden)

    Klink Björn U

    2010-10-01

    Full Text Available Abstract Background In kinetic crystallography, the usually static method of X-ray diffraction is expanded to allow time-resolved analysis of conformational rearrangements in protein structures. To achieve this, reactions have to be triggered within the protein crystals of interest, and optical spectroscopy can be used to monitor the reaction state. For this approach, a modified form of H-Ras p21 was designed which allows reaction initiation and fluorescence readout of the initiated GTPase reaction within the crystalline state. Rearrangements within the crystallized protein due to the progressing reaction and associated heterogeneity in the protein conformations have to be considered in the subsequent refinement processes. Results X-ray diffraction experiments on H-Ras p21 in different states along the reaction pathway provide detailed information about the kinetics and mechanism of the GTPase reaction. In addition, a very high data quality of up to 1.0 Å resolution allowed distinguishing two discrete subconformations of H-Ras p21, expanding the knowledge about the intrinsic flexibility of Ras-like proteins, which is important for their function. In a complex of H-Ras•GppNHp (guanosine-5'-(β,γ-imido-triphosphate, a second Mg2+ ion was found to be coordinated to the γ-phosphate group of GppNHp, which positions the hydrolytically active water molecule very close to the attacked γ-phosphorous atom. Conclusion For the structural analysis of very high-resolution data we have used a new 'two-chain-isotropic-refinement' strategy. This refinement provides an alternative and easy to interpret strategy to reflect the conformational variability within crystal structures of biological macromolecules. The presented fluorescent form of H-Ras p21 will be advantageous for fluorescence studies on H-Ras p21 in which the use of fluorescent nucleotides is not feasible.

  17. Combination of X-ray crystallography, SAXS and DEER to obtain the structure of the FnIII-3, 4 domains of integrin α6β4

    Energy Technology Data Exchange (ETDEWEB)

    Alonso-García, Noelia [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); García-Rubio, Inés [ETH Zürich, Vladimir-Prelog-Weg 2, CH-8093 Zürich (Switzerland); Academia General Militar, Carretera de Huesca s/n, 50090 Zaragoza (Spain); Manso, José A. [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); Buey, Rubén M. [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); Urien, Hector [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain); Sonnenberg, Arnoud [Netherlands Cancer Institute, Plesmanlaan 121, 1066 CX Amsterdam (Netherlands); Jeschke, Gunnar [ETH Zürich, Vladimir-Prelog-Weg 2, CH-8093 Zürich (Switzerland); Pereda, José M. de, E-mail: pereda@usal.es [Consejo Superior de Investigaciones Científicas – University of Salamanca, Campus Unamuno, 37007 Salamanca (Spain)

    2015-04-01

    The structure of the FnIII-3, 4 region of integrin β4 was solved using a hybrid approach that combines crystallographic structures, SAXS, DEER and molecular modelling. The structure helps in understanding how integrin β4 might bind to other hemidesmosomal proteins and mediate signalling. Integrin α6β4 is a major component of hemidesmosomes that mediate the stable anchorage of epithelial cells to the underlying basement membrane. Integrin α6β4 has also been implicated in cell proliferation and migration and in carcinoma progression. The third and fourth fibronectin type III domains (FnIII-3, 4) of integrin β4 mediate binding to the hemidesmosomal proteins BPAG1e and BPAG2, and participate in signalling. Here, it is demonstrated that X-ray crystallography, small-angle X-ray scattering and double electron–electron resonance (DEER) complement each other to solve the structure of the FnIII-3, 4 region. The crystal structures of the individual FnIII-3 and FnIII-4 domains were solved and the relative arrangement of the FnIII domains was elucidated by combining DEER with site-directed spin labelling. Multiple structures of the interdomain linker were modelled by Monte Carlo methods complying with DEER constraints, and the final structures were selected against experimental scattering data. FnIII-3, 4 has a compact and cambered flat structure with an evolutionary conserved surface that is likely to correspond to a protein-interaction site. Finally, this hybrid method is of general application for the study of other macromolecules and complexes.

  18. Elucidation of Lipid Binding Sites on Lung Surfactant Protein A Using X-ray Crystallography, Mutagenesis, and Molecular Dynamics Simulations.

    Science.gov (United States)

    Goh, Boon Chong; Wu, Huixing; Rynkiewicz, Michael J; Schulten, Klaus; Seaton, Barbara A; McCormack, Francis X

    2016-07-01

    Surfactant protein A (SP-A) is a collagenous C-type lectin (collectin) that is critical for pulmonary defense against inhaled microorganisms. Bifunctional avidity of SP-A for pathogen-associated molecular patterns (PAMPs) such as lipid A and for dipalmitoylphosphatidylcholine (DPPC), the major component of surfactant membranes lining the air-liquid interface of the lung, ensures that the protein is poised for first-line interactions with inhaled pathogens. To improve our understanding of the motifs that are required for interactions with microbes and surfactant structures, we explored the role of the tyrosine-rich binding surface on the carbohydrate recognition domain of SP-A in the interaction with DPPC and lipid A using crystallography, site-directed mutagenesis, and molecular dynamics simulations. Critical binding features for DPPC binding include a three-walled tyrosine cage that binds the choline headgroup through cation-π interactions and a positively charged cluster that binds the phosphoryl group. This basic cluster is also critical for binding of lipid A, a bacterial PAMP and target for SP-A. Molecular dynamics simulations further predict that SP-A binds lipid A more tightly than DPPC. These results suggest that the differential binding properties of SP-A favor transfer of the protein from surfactant DPPC to pathogen membranes containing appropriate lipid PAMPs to effect key host defense functions. PMID:27324153

  19. Sample Injector Fabrication and Delivery Method Development for Serial Crystallography using Synchrotrons and X-ray Free Electron Lasers

    Science.gov (United States)

    Nelson, Garrett Charles

    Sample delivery is an essential component in biological imaging using serial diffraction from X-ray Free Electron Lasers (XFEL) and synchrotrons. Recent developments have made possible the near-atomic resolution structure determination of several important proteins, including one G protein-coupled receptor (GPCR) drug target, whose structure could not easily have been determined otherwise (Appendix A). In this thesis I describe new sample delivery developments that are paramount to advancing this field beyond what has been accomplished to date. Soft Lithography was used to implement sample conservation in the Gas Dynamic Virtual Nozzle (GDVN). A PDMS/glass composite microfluidic injector was created and given the capability of millisecond fluidic switching of a GDVN liquid jet within the divergent section of a 2D Laval-like GDVN nozzle, providing a means of collecting sample between the pulses of current XFELs. An oil/water droplet immersion jet was prototyped that suspends small sample droplets within an oil jet such that the sample droplet frequency may match the XFEL pulse repetition rate. A similar device was designed to use gas bubbles for synchronized "on/off" jet behavior and for active micromixing. 3D printing based on 2-Photon Polymerization (2PP) was used to directly fabricate reproducible GDVN injectors at high resolution, introducing the possibility of systematic nozzle research and highly complex GDVN injectors. Viscous sample delivery using the "LCP injector" was improved with a method for dealing with poorly extruding sample mediums when using full beam transmission from the Linac Coherent Light Source (LCLS), and a new viscous crystal-carrying medium was characterized for use in both vacuum and atmospheric environments: high molecular weight Polyethylene Glycol.

  20. SPECTROSCOPY STUDIES, X-RAY CRYSTALLOGRAPHY, AND ANTITUMOR EVALUATION OF THE BEHAVIOR OF REACTIONS OF BISDIMEDONE DERIVATIVES WITH MALONONITRILE OR WITH BENZYLIDENEMALONONITILE IN ETHANOLIC PIPERIDINE

    Directory of Open Access Journals (Sweden)

    Fatima Al-Omran

    2014-03-01

    Full Text Available A simple, environmentally acceptable, a one-pot method, which is efficient, inexpensive, and rapid, afforded excellent yields of the 4H-chromeme derivatives 5 and 6 from a three-component reaction of dimedone, arylaldehdes 2a-b, and malononitrile and a two-component reaction of bisdimedones 3a-b and malononitrile, respectively. Refluxing ethanolic piperidine was used as the catalyst for the 10-min reactions. A one-pot reaction of benzylidenemalononitrile, instead of malononitrile, with bisdimedones 3a-b, using the aforementioned reaction, also provided the 4H-chromene derivative 5 in excellent yield. The structures of the newly synthesized compounds were elucidated by elemental analyses, X-ray crystallography, and a variety of spectroscopic methods, including proton and carbon nuclear magnetic resonance spectroscopy (1H-NMR and 13C-NMR, respectively, correlation spectroscopy (COSY, heteronuclear single quantum coherence spectroscopy (HSQC, heteronuclear multiple-bond correlation spectroscopy (HMBC, and mass spectrometry (MS. The inhibitory effects of the 4H-chromeme derivatives 5 and 6 on the in vitro growth of human tumor cell and normal cell lines were greater than that of the reference drug doxorubicin.

  1. Measuring the x-ray resolving power of bent potassium acid phthalate diffraction crystalsa)

    Science.gov (United States)

    Haugh, M. J.; Wu, M.; Jacoby, K. D.; Loisel, G. P.

    2014-11-01

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories in Albuquerque, New Mexico. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a double crystal diffractometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  2. Measuring the X-ray Resolving Power of Bent Potassium Acid Phthalate Diffraction Crystals

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, M. J. [NSTec; Wu, M. [SNL; Jacoby, K. D. [NSTec; Loisel, G. P. [SNL

    2014-11-01

    This report presents the results from measuring the X-ray resolving power of a curved potassium acid phthalate (KAP(001)) spectrometer crystal using two independent methods. It is part of a continuing effort to measure the fundamental diffraction properties of bent crystals that are used to study various characteristics of high temperature plasmas. Bent crystals like KAP(001) do not usually have the same diffraction properties as corresponding flat crystals. Models that do exist to calculate the effect of bending the crystal on the diffraction properties have simplifying assumptions and their accuracy limits have not been adequately determined. The type of crystals that we measured is being used in a spectrometer on the Z machine at Sandia National Laboratories (SNL) in Albuquerque, NM. The first technique for measuring the crystal resolving power measures the X-ray spectral line width of the characteristic lines from several metal anodes. The second method uses a diode X-ray source and a dual goniometer arrangement to measure the reflectivity curve of the KAP(001) crystal. The width of that curve is inversely proportional to the crystal resolving power. The measurement results are analyzed and discussed.

  3. Mapping the topographic epitope landscape on the urokinase plasminogen activator receptor (uPAR by surface plasmon resonance and X-ray crystallography

    Directory of Open Access Journals (Sweden)

    Baoyu Zhao

    2015-12-01

    Full Text Available The urokinase-type plasminogen activator receptor (uPAR or CD87 is a glycolipid-anchored membrane protein often expressed in the microenvironment of invasive solid cancers and high levels are generally associated with poor patient prognosis (Kriegbaum et al., 2011 [1]. uPAR is organized as a dynamic modular protein structure composed of three homologous Ly6/uPAR domains (LU.This internally flexible protein structure of uPAR enables an allosteric regulation of the interactions with its two principal ligands: the serine protease urokinase-type plasminogen activator (uPA and the provisional matrix protein vitronectin (Vn (Mertens et al., 2012; Gårdsvoll et al., 2011; Madsen et al., 2007 [2–4]. The data presented here relates to the non-covalent trapping of one of these biologically relevant uPAR-conformations by a novel class of monoclonal antibodies (Zhao et al., 2015 [5] and to the general mapping of the topographic epitope landscape on uPAR. The methods required to achieve these data include: (1 recombinant expression and purification of a uPAR-hybrid protein trapped in the desired conformation [patent; WO 2013/020898 A12013]; (2 developing monoclonal antibodies with unique specificities using this protein as antigen; (3 mapping the functional epitope on uPAR for these mAbs by surface plasmon resonance with a complete library of purified single-site uPAR mutants (Zhao et al., 2015; Gårdsvoll et al., 2006 [5,6]; and finally (4 solving the three-dimensional structures for one of these mAbs by X-ray crystallography alone and in complex with uPAR [deposited in the PDB database as 4QTH and 4QTI, respectively].

  4. Mapping the topographic epitope landscape on the urokinase plasminogen activator receptor (uPAR) by surface plasmon resonance and X-ray crystallography.

    Science.gov (United States)

    Zhao, Baoyu; Gandhi, Sonu; Yuan, Cai; Luo, Zhipu; Li, Rui; Gårdsvoll, Henrik; de Lorenzi, Valentina; Sidenius, Nicolai; Huang, Mingdong; Ploug, Michael

    2015-12-01

    The urokinase-type plasminogen activator receptor (uPAR or CD87) is a glycolipid-anchored membrane protein often expressed in the microenvironment of invasive solid cancers and high levels are generally associated with poor patient prognosis (Kriegbaum et al., 2011 [1]). uPAR is organized as a dynamic modular protein structure composed of three homologous Ly6/uPAR domains (LU).This internally flexible protein structure of uPAR enables an allosteric regulation of the interactions with its two principal ligands: the serine protease urokinase-type plasminogen activator (uPA) and the provisional matrix protein vitronectin (Vn) (Mertens et al., 2012; Gårdsvoll et al., 2011; Madsen et al., 2007 [2-4]). The data presented here relates to the non-covalent trapping of one of these biologically relevant uPAR-conformations by a novel class of monoclonal antibodies (Zhao et al., 2015 [5]) and to the general mapping of the topographic epitope landscape on uPAR. The methods required to achieve these data include: (1) recombinant expression and purification of a uPAR-hybrid protein trapped in the desired conformation [patent; WO 2013/020898 A12013]; (2) developing monoclonal antibodies with unique specificities using this protein as antigen; (3) mapping the functional epitope on uPAR for these mAbs by surface plasmon resonance with a complete library of purified single-site uPAR mutants (Zhao et al., 2015; Gårdsvoll et al., 2006 [5,6]); and finally (4) solving the three-dimensional structures for one of these mAbs by X-ray crystallography alone and in complex with uPAR [deposited in the PDB database as 4QTH and 4QTI, respectively]. PMID:26504891

  5. Structures of Plutonium(IV) and Uranium(VI) with N,N-Dialkyl Amides from Crystallography, X-ray Absorption Spectra, and Theoretical Calculations.

    Science.gov (United States)

    Acher, Eléonor; Hacene Cherkaski, Yanis; Dumas, Thomas; Tamain, Christelle; Guillaumont, Dominique; Boubals, Nathalie; Javierre, Guilhem; Hennig, Christoph; Solari, Pier Lorenzo; Charbonnel, Marie-Christine

    2016-06-01

    The structures of plutonium(IV) and uranium(VI) ions with a series of N,N-dialkyl amides ligands with linear and branched alkyl chains were elucidated from single-crystal X-ray diffraction (XRD), extended X-ray absorption fine structure (EXAFS), and theoretical calculations. In the field of nuclear fuel reprocessing, N,N-dialkyl amides are alternative organic ligands to achieve the separation of uranium(VI) and plutonium(IV) from highly concentrated nitric acid solution. EXAFS analysis combined with XRD shows that the coordination structure of U(VI) is identical in the solution and in the solid state and is independent of the alkyl chain: two amide ligands and four bidentate nitrate ions coordinate the uranyl ion. With linear alkyl chain amides, Pu(IV) also adopt identical structures in the solid state and in solution with two amides and four bidentate nitrate ions. With branched alkyl chain amides, the coordination structure of Pu(IV) was more difficult to establish unambiguously from EXAFS. Density functional theory (DFT) calculations were consequently performed on a series of structures with different coordination modes. Structural parameters and Debye-Waller factors derived from the DFT calculations were used to compute EXAFS spectra without using fitting parameters. By using this methodology, it was possible to show that the branched alkyl chain amides form partly outer-sphere complexes with protonated ligands hydrogen bonded to nitrate ions. PMID:27171842

  6. Site-specific Incorporation of 3-Iodo-L-tyrosine into Proteins and Single-wavelength Anomalous Dispersion Phasing with Soft X-ray in Protein Crystallography

    Science.gov (United States)

    Murayama, Kazutaka; Sakamoto, Kensaku

    Iodine is a good anomalous scatter for radiations from in-house X-ray generators (Cu/CrKα). Non-natural amino acid, 3-iodo-L-tyrosine, is able to be site-specifically incorporated into proteins with amber suppresser tRNA and mutated TyrRS from M. jannaschii in the E. coli expression system. To determine the crystal structure of acetyl transferase from T. thermophilus, iodotyrosine-containing proteins were prepared and crystallized. Structure determination was successfully conducted with the protein variant with iodotyrosine at position 111. Anomalous signals from iodotyrosine with Cu/CrKα radiations were both sufficient to calculate clear electron density map. In the crystal structure, iodotyrosine did not significantly disturb the native structure.

  7. Electronic structure of aromatic amino acids studied by soft x-ray spectroscopy

    Science.gov (United States)

    Zhang, Wenhua; Carravetta, Vincenzo; Plekan, Oksana; Feyer, Vitaliy; Richter, Robert; Coreno, Marcello; Prince, Kevin C.

    2009-07-01

    The electronic structure of phenylalanine, tyrosine, tryptophan, and 3-methylindole in the gas phase was investigated by x-ray photoemission spectroscopy (XPS) and near edge x-ray absorption fine structure (NEXAFS) spectroscopy at the C, N, and O K-edges. The XPS spectra have been calculated for the four principal conformers of each amino acid, and the spectra weighted by the Boltzmann population ratios calculated from published free energies. Instead of the single peaks expected from the stoichiometry of the compounds, the N 1s core level spectra of phenylalanine and tryptophan show features indicating that more than one conformer is present. The calculations reproduce the experimental features. The C and O 1s spectra do not show evident effects due to conformational isomerism. The calculations predict that such effects are small for carbon, and for oxygen it appears that only broadening occurs. The carbon K-edge NEXAFS spectra of these aromatic amino acids are similar to the published data of the corresponding molecules in the solid state, but show more structure due to the higher resolution in the present study. The N K-edge spectra of tryptophan and 3-methylindole differ from phenylalanine and tyrosine, as the first two both contain a nitrogen atom located in a pyrrole ring. The nitrogen K-edge NEXAFS spectra of aromatic amino acids do not show any measurable effects due to conformational isomerism, in contrast to the photoemission results. Calculations support this result and show that variations of the vertical excitation energies of different conformers are small, and cannot be resolved in the present experiment. The O NEXAFS spectra of these three aromatic compounds are very similar to other, simpler amino acids, which have been studied previously.

  8. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    International Nuclear Information System (INIS)

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis (YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability (Rwork = 16.2, Rfree = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh

  9. Exploring the Mechanism of β-Lactam Ring Protonation in the Class A β-lactamase Acylation Mechanism Using Neutron and X-ray Crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Vandavasi, Venu Gopal; Weiss, Kevin L.; Cooper, Jonathan B.; Erskine, Peter T.; Tomanicek, Stephen J.; Ostermann, Andreas; Schrader, Tobias E.; Ginell, Stephan L.; Coates, Leighton

    2016-01-14

    The catalytic mechanism of class A beta-lactamases is often debated due in part to the large number of amino acids that interact with bound beta-lactam substrates. The role and function of the conserved residue Lys 73 in the catalytic mechanism of class A type beta-lactamase enzymes is still not well understood after decades of scientific research. To better elucidate the functions of this vital residue, we used both neutron and high-resolution X-ray diffraction to examine both the structures of the ligand free protein and the acyl-enzyme complex of perdeuterated E166A Toho-1 beta-lactamase with the antibiotic cefotaxime. The E166A mutant lacks a critical glutamate residue that has a key role in the deacylation step of the catalytic mechanism, allowing the acyl-enzyme adduct to be captured for study. In our ligand free structures, Lys 73 is present in a single conformation, however in all of our acyl-enzyme structures, Lys 73 is present in two different conformations, in which one conformer is closer to Ser 70 while the other conformer is positioned closer to Ser 130, which supports the existence of a possible pathway by which proton transfer from Lys 73 to Ser 130 can occur. This and further clarifications of the role of Lys 73 in the acylation mechanism may facilitate the design of inhibitors that capitalize on the enzymes native machinery.

  10. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    Energy Technology Data Exchange (ETDEWEB)

    Balaev, V. V.; Lashkov, A. A., E-mail: alashkov83@gmail.com; Gabdoulkhakov, A. G.; Seregina, T. A.; Dontsova, M. V.; Mikhailov, A. M. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2015-03-15

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis (YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability (R{sub work} = 16.2, R{sub free} = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh.

  11. Osmium(III) analogues of KP1019: Electrochemical and chemical synthesis, spectroscopic characterization, x-ray crystallography, hydrolytic stability, and antiproliferative activity

    KAUST Repository

    Kuhn, Paul-Steffen

    2014-10-20

    A one-electron reduction of osmium(IV) complexes trans-[OsIVCl4(Hazole)2], where Hazole = 1H-pyrazole ([1]0), 2H-indazole ([2]0), 1H-imidazole ([3]0), and 1H-benzimidazole ([4]0), afforded a series of eight new complexes as osmium analogues of KP1019, a lead anticancer drug in clinical trials, with the general formula (cation)[trans-OsIIICl4(Hazole)2], where cation = H2pz+ (H2pz[1]), H2ind+ (H2ind[2]), H2im+ (H2im[3]), Ph4P+ (Ph4P[3]), nBu4N+ (nBu4N[3]), H2bzim+ (H2bzim[4]), Ph4P+ (Ph4P[4]), and nBu4N+ (nBu4N[4]). All complexes were characterized by elemental analysis, 1H NMR spectroscopy, electrospray ionization mass spectrometry, UV-vis spectroscopy, cyclic voltammetry, while H2pz[1], H2ind[2], and nBu4[3], in addition, by X-ray diffraction. The reduced species [1]- and [4]- are stable in aqueous media in the absence of air oxygen and do not react with small biomolecules such as amino acids and the nucleotide 5′-dGMP. Cell culture experiments in five different human cancer cell lines (HeLa, A549, FemX, MDA-MB-453, and LS-174) and one noncancerous cell line (MRC-5) were performed, and the results were discussed and compared to those for KP1019 and cisplatin. Benzannulation in complexes with similar structure enhances antitumor activity by several orders of magnitude, implicating different mechanisms of action of the tested compounds. In particular, complexes H2ind[2] and H2bzim[4] exhibited significant antiproliferative activity in vitro when compared to H2pz[1] and H2im[3]. (Chemical Equation Presented).

  12. X-ray-induced photo-chemistry and X-ray absorption spectroscopy of biological samples

    OpenAIRE

    George, Graham N.; Pickering, Ingrid J.; Pushie, M. Jake; Nienaber, Kurt; Hackett, Mark J.; Ascone, Isabella; Hedman, Britt; Hodgson, Keith O.; Aitken, Jade B.; Levina, Aviva; Glover, Christopher; Lay, Peter A.

    2012-01-01

    X-ray-induced photo-chemistry of metal sites within biological molecules is a concern for X-ray absorption spectroscopy, X-ray crystallography and other techniques in which samples are illuminated with X-rays. The effects of X-ray-induced photo-chemistry are reviewed and the methods used to mitigate these in X-ray absorption spectroscopy are outlined.

  13. Silica-supported silicotungstic acid: A study by X-ray photoelectron spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Berry, Frank J.; Derrick, Glyn R. [Department of Chemistry and Analytical Sciences, Robert Hooke Building, Open University, Walton Hall, Milton Keynes, MK7 6AA (United Kingdom); Marco, Jose F. [Instituto de Quimica -Fisica ' Rocasolano' , Consejo Superior de Investigaciones Cientificas, Serrano 119, 28006 Madrid (Spain); Mortimer, Michael [Department of Chemistry and Analytical Sciences, Robert Hooke Building, Open University, Walton Hall, Milton Keynes, MK7 6AA (United Kingdom)], E-mail: m.mortimer@open.ac.uk

    2009-04-15

    W 4f and O 1s X-ray photoelectron spectra for silicotungstic acid, H{sub 4}SiW{sub 12}O{sub 40}, in pure and silica-supported form are reported. W 4f XP spectra for the supported acid are analysed in terms of contributions from two W(VI) spin-orbit doublets arising from tungsten atoms in terminal W=O bonds some of which directly interact with the silica surface. At low loading (3.2 wt.%) significant changes in the relative contributions and binding energies of the two spin-orbit doublets are taken as evidence of a strong interaction of individual [SiW{sub 12}O{sub 40}]{sup 4-} anions with highly active sites on the silica surface. It is suggested that selective ordering of silanol groups can occur on the silica surface in order to accommodate the adsorption of individual [SiW{sub 12}O{sub 40}]{sup 4-} anions.

  14. A new small-angle X-ray scattering set-up on the crystallography beamline I711 at MAX-lab

    DEFF Research Database (Denmark)

    Knaapila, M.; Svensson, C.; Barauskas, J.;

    2009-01-01

    A small-angle X-ray scattering (SAXS) set-up has recently been developed at beamline I711 at the MAX II storage ring in Lund (Sweden). An overview of the required modifications is presented here together with a number of application examples. The accessible q range in a SAXS experiment is 0.009-0...

  15. X-ray Excited Optical Fluorescence and Diffraction Imaging of Reactivity and Crystallinity in a Zeolite Crystal: Crystallography and Molecular Spectroscopy in One.

    Science.gov (United States)

    Ristanović, Zoran; Hofmann, Jan P; Richard, Marie-Ingrid; Jiang, Tao; Chahine, Gilbert A; Schülli, Tobias U; Meirer, Florian; Weckhuysen, Bert M

    2016-06-20

    Structure-activity relationships in heterogeneous catalysis are challenging to be measured on a single-particle level. For the first time, one X-ray beam is used to determine the crystallographic structure and reactivity of a single zeolite crystal. The method generates μm-resolved X-ray diffraction (μ-XRD) and X-ray excited optical fluorescence (μ-XEOF) maps of the crystallinity and Brønsted reactivity of a zeolite crystal previously reacted with a styrene probe molecule. The local gradients in chemical reactivity (derived from μ-XEOF) were correlated with local crystallinity and framework Al content, determined by μ-XRD. Two distinctly different types of fluorescent species formed selectively, depending on the local zeolite crystallinity. The results illustrate the potential of this approach to resolve the crystallographic structure of a porous material and its reactivity in one experiment via X-ray induced fluorescence of organic molecules formed at the reactive centers. PMID:27145171

  16. Soft X-Ray Spectromicroscopy Investigation of the Interaction of Aquatic Humic Acid and Clay Colloids.

    Science.gov (United States)

    Rothe; Denecke; Dardenne

    2000-11-01

    Soft X-ray spectromicroscopy investigations of the interaction of aquatic humic acid (HA) and montmorillonite colloids have been performed in situ at the NSLS X1-A STXM endstation. Images have been recorded of montmorillonite particles, HA aggregates, and mixed suspensions of both montmorillonite + HA and montmorillonite + carboxyl polystyrene microspheres, as reference organic colloids. Special emphasis has been placed on the sample preparation technique in order to keep the colloid particles hydrated during all measurements. C 1s near edge absorption fine structure extracted from STXM image stacks reveals electronic transitions corresponding to functional -COOH and -C(6)H(5) groups present in HA and polystyrene. XANES peak intensities reflect the relative amounts of these two carbon functional groups in the organic particles. For example, the greater amount of carboxyl groups in HA compared to the latex reference particles affects a larger 1s-->pi* transition intensity. A specific form of montmorillonite-HA particle agglomeration at near-neutral pH has been observed. Under these conditions, we found no separate clustering of HA. Instead, STXM images show the HA to coat the clay mineral surface, leading to nearly a fractal manner of aggregation. Copyright 2000 Academic Press.

  17. Oil-free hyaluronic acid matrix for serial femtosecond crystallography

    Science.gov (United States)

    Sugahara, Michihiro; Song, Changyong; Suzuki, Mamoru; Masuda, Tetsuya; Inoue, Shigeyuki; Nakane, Takanori; Yumoto, Fumiaki; Nango, Eriko; Tanaka, Rie; Tono, Kensuke; Joti, Yasumasa; Kameshima, Takashi; Hatsui, Takaki; Yabashi, Makina; Nureki, Osamu; Numata, Keiji; Iwata, So

    2016-04-01

    The grease matrix was originally introduced as a microcrystal-carrier for serial femtosecond crystallography and has been expanded to applications for various types of proteins, including membrane proteins. However, the grease-based matrix has limited application for oil-sensitive proteins. Here we introduce a grease-free, water-based hyaluronic acid matrix. Applications for proteinase K and lysozyme proteins were able to produce electron density maps at 2.3-Å resolution.

  18. Electron Crystallography of Aquaporins

    OpenAIRE

    Andrews, Simeon; Reichow, Steve L; Gonen, Tamir

    2008-01-01

    Aquaporins are a family of ubiquitous membrane proteins that form a pore for the permeation of water. Both electron and X-ray crystallography played major roles in determining the atomic structures of a number of aquaporins. This review focuses on electron crystallography, and its contribution to the field of aquaporin biology. We briefly discuss electron crystallography and the two-dimensional crystallization process. We describe features of aquaporins common to both electron and X-ray cryst...

  19. Azo coupling of 4-nitrophenyldiazonium chloride with aliphatic nucleophiles: an integrated organic synthesis and X-ray crystallography experiment; Acoplamento de cloreto de 4-nitrofenildiazonio com nucleofilos alifaticos: experimento integrado de sintese organica e cristalografia de raios X

    Energy Technology Data Exchange (ETDEWEB)

    Cunha, Silvio; Marques, Monique F.; Rocha, Valeria, E-mail: silviodc@ufba.br [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Instituto de Quimica; Lariucci, Carlito; Vencato, Ivo [Universidade Federal de Goiania (UFG), GO (Brazil). Instituto de Fisica

    2013-11-01

    This article describes an undergraduate experiment for the synthesis of p-nitrophenyldiazonium chloride and its coupling with acetylacetone and two enaminones, 4-phenylamino-pent-3-en-2-one and 4-amino-pent-3-en-2-one, in an adaptation of a previously reported synthetic protocol. The azo dyes 4-(E)-phenylamino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one and 4-(E)-amino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one were obtained, and the solid state structure of this latter azo compound was characterized by single crystal X-ray diffraction studies. This two-week integrated laboratory approach involves simple synthetic experiments and microwave chemistry in the organic laboratory plus crystallography analysis, suitable for novice students on undergraduate experimental chemistry courses. (author)

  20. X-ray investigation of gene-engineered human insulin crystallized from a solution containing polysialic acid

    Science.gov (United States)

    Timofeev, V. I.; Chuprov-Netochin, R. N.; Samigina, V. R.; Bezuglov, V. V.; Miroshnikov, K. A.; Kuranova, I. P.

    2010-01-01

    Attempts to crystallize the noncovalent complex of recombinant human insulin with polysialic acid were carried out under normal and microgravity conditions. Both crystal types belonged to the same space group, I213, with unit-cell parameters a = b = c = 77.365 Å, α = β = γ = 90.00°. The reported space group and unit-cell parameters are almost identical to those of cubic insulin reported in the PDB. The results of X-ray studies confirmed that the crystals obtained were cubic insulin crystals and that they contained no polysialic acid or its fragments. Electron-density maps were calculated using X-ray diffraction sets from earth-grown and microgravity-grown crystals and the three-dimensional structure of the insulin molecule was determined and refined. The conformation and secondary-structural elements of the insulin molecule in different crystal forms were compared. PMID:20208155

  1. Synthesis, X-ray crystallography, spectroscopic (FT-IR, 1H &13C NMR and UV), computational (DFT/B3LYP) and enzymes inhibitory studies of 7-hydroximinocholest-5-en-3-ol acetate

    Science.gov (United States)

    Ahmad, Faheem; Parveen, Mehtab; Alam, Mahboob; Azaz, Shaista; Malla, Ali Mohammed; Alam, Mohammad Jane; Lee, Dong-Ung; Ahmad, Shabbir

    2016-07-01

    The present study reports the synthesis of 7-Hydroximinocholest-5-en-3-ol acetate (syn. 3β-acetoxycholest-5-en-7-one oxime; in general, steroidal oxime). The identity of steroidal molecule was confirmed by NMR, FT-IR, MS, CHN microanalysis and X-ray crystallography. DFT calculations on the titled molecule have been performed. The molecular structure and spectra interpreted by Gaussian hybrid computational analysis theory (B3LYP) are found to be in good correlation with the experimental data obtained from the various spectrophotometric techniques. The vibrational bands appearing in the FTIR are assigned with great accuracy using harmonic frequencies along with intensities and animated modes. Molecular properties like HOMO-LUMO analysis, chemical reactivity descriptors, MEP mapping, dipole moment and natural atomic charges have been presented at the same level of theory. Moreover, the Hirshfeld analysis was carried out to ascertain the secondary interactions and associated 2D fingerprint plots. The percentages of various interactions are pictorialized by fingerprint plots of Hirshfeld surface. Steroidal oxime exhibited promising inhibitory activity against acetylcholinesterase (AChE) as compared to the reference drug, tacrine. Molecular docking was performed to introduce steroidal molecules into the X-ray crystal structures of acetylcholinesterase at the active site to find out the probable binding mode. The results of molecular docking admitted that steroidal oxime may exhibit enzyme inhibitor activity.

  2. Titration of a Solid Acid Monitored by X-Ray Diffraction

    Science.gov (United States)

    Dungey, Keenan E.; Epstein, Paul

    2007-01-01

    An experiment is described to introduce students to an important class of solid-state reactions while reinforcing concepts of titration by using a pH meter and a powder X-ray diffractometer. The experiment was successful in teaching students the abstract concepts of solid-state structure and diffraction by applying the diffraction concepts learned…

  3. Auger electron and X-ray photoelectron spectroscopic study of the biocorrosion of copper by alginic acid polysaccharide

    Science.gov (United States)

    Jolley, John G.; Geesey, Gill G.; Hankins, Michael R.; Wright, Randy B.; Wichlacz, Paul L.

    1989-08-01

    Thin films (3.4 nm) of copper on germanium substrates were exposed to 2% alginic acid polysaccharide aqueous solution. Pre- and post-exposure characterization were done by Auger electron spectroscopy and X-ray photoelectron spectroscopy. Ancillary graphite furnace atomic absorption spectroscopy was used to monitor the removal process of the copper thin film from the germanium substrate. Results indicate that some of the copper was oxidized by the alginic acid solution. Some of the copper was removed from the Cu/Ge interface and incorporated into the polymer matrix. Thus, biocorrosion of copper was exhibited by the alginic acid polysaccharide.

  4. Intergrown new zeolite beta polymorphs with interconnected 12-ring channels solved by combining electron crystallography and single-crystal X-ray diffraction

    KAUST Repository

    Yu, Zhengbao

    2012-10-09

    Two new polymorphs of zeolite beta, denoted as SU-78A and SU-78B, were synthesized by employing dicyclohexylammonium hydroxides as organic structure-directing agents. The structure was solved by combining transmission electron microscopy and single-crystal X-ray diffraction. SU-78 is an intergrowth of SU-78A and SU-78B and contains interconnected 12-ring channels in three directions. The two polymorphs are built from the same building layer, similar to that for the zeolite beta family. The layer stacking in SU-78, however, is different from those in zeolite beta polymorph A, B, and C, showing new zeolite framework topologies. SU-78 is thermally stable up to 600 °C. © 2012 American Chemical Society.

  5. Structural investigation of (2E)-2-(ethoxycarbonyl)-3-[(4-methoxyphenyl)amino]prop-2-enoic acid: X-ray crystal structure, spectroscopy and DFT

    Science.gov (United States)

    Venkatesan, Perumal; Rajakannan, Venkatachalam; Venkataramanan, Natarajan S.; Ilangovan, Andivelu; Sundius, Tom; Thamotharan, Subbiah

    2016-09-01

    The title compound, (2E)-2-(ethoxycarbonyl)-3-[(4-methoxyphenyl)amino]prop-2-enoic acid is characterized by means of X-ray crystallography, spectroscopic methods and quantum chemical calculations. The title compound crystallizes in centrosymmetric space group P21/c. Moreover, the crystal structure is primarily stabilized through intramolecular Nsbnd H⋯O and Osbnd H⋯O and intermolecular Nsbnd H⋯O and Csbnd H⋯O interactions along with carbonyl⋯carbonyl and Csbnd H⋯C contacts. These intermolecular interactions are analysed and quantified by using Hirshfeld surface analysis, PIXEL energy, NBO, AIM and DFT calculations. The overall lattice energies of the title and parent compounds suggest that the title compound is stabilized by a 4.5 kcal mol-1 higher energy than the parent compound. The additional stabilization force comes from the methoxy substitution on the title molecule, which is evident since the methoxy group is involved in the intermolecular Csbnd H⋯O interaction as an acceptor. The vibrational modes of the interacting groups are investigated using both experimental and theoretical FT-IR and FT-Raman spectra. The experimental and theoretical UV-Vis spectra agree well. The time dependent DFT spectra show that the ligand-to-ligand charge transfer is responsible for the intense absorbance of the compound.

  6. Nucleic acid fragmentation on the millisecond timescale using a conventional X-ray rotating anode source: application to protein–DNA footprinting

    OpenAIRE

    Henn, Arnon; Halfon, Jacob; Kela, Itai; Orion, Itzhak; Sagi, Irit

    2001-01-01

    Nucleic acid fragmentation (footprinting) by ·OH radicals is used often as a tool to probe nucleic acid structure and nucleic acid–protein interactions. This method has proven valuable because it provides structural information with single base pair resolution. Recent developments in the field introduced the ‘synchrotron X-ray footprinting’ method, which uses a high-flux X-ray source to produce single base pair fragmentation of nucleic acid in tens of milliseconds. We developed a complementar...

  7. X-Ray Characterisation of Various Aluminium Phases in the Medicinal Herb Bacopa Monnieri Affected by Simulated Acid Rain

    OpenAIRE

    Mallick, B.

    2012-01-01

    In the present investigation various aluminium-based new phases formed due to substitution of sulphur via simulated acid rain in Bacopa monnieri have been analyzed using X-ray diffraction (XRD) technique. So far there is no report on the effects of acid rain on the B. monnieri herb and its vital properties like memory-boosting mechanism. Therefore, in the present study, an attempt has been made to analyze the various aluminium phase (salt) formations due to the substitution of sulphur via sim...

  8. X-ray Crystallography, DFT Calculations and Molecular Docking of Indole-Arylpiperazine Derivatives as α1A-Adrenoceptor Antagonists

    Directory of Open Access Journals (Sweden)

    Wei Xu

    2015-10-01

    Full Text Available Indole-arylpiperazine derivatives have exhibited good selectivity for the α1A-adrenoceptor, but the structure-activity-binding mechanism relationship remains unclear. In the current study, three compounds (1, 2 and 3 were investigated through single-crystal X-ray diffraction analysis, density functional theory (DFT calculations and molecular docking using a homology model of the α1A receptor. Compounds 1 and 3 form H-bonds networks to stabilize their three-dimensional structures, while C–H···π interactions play a significant role in the packing of 2. Based on DFT-optimized conformations, the HOMO-LUMO energy gaps and molecular electrostatic potential (MEP were theoretically calculated at the B3LYP/6-311G (d, p level of theory. Chemical reactivity increases in the order of 3 < 2 < 1, and the maximum positive region of the MEP maps is mainly localized over the NH group. The binding mechanisms of ligand-α1A-adrenoceptor complexes were illustrated by molecular docking. Binding to Gln177 of the second extracellular loop region via hydrogen bonds is likely to be essential for α1A-selective antagonists. The present work sheds light on the studies of structure-activity-binding mechanism and aids in the design of α1A antagonists with high selectivity.

  9. Novel protein-inhibitor interactions in site 3 of Ca(2+)-bound S100B as discovered by X-ray crystallography.

    Science.gov (United States)

    Cavalier, Michael C; Melville, Zephan; Aligholizadeh, Ehson; Raman, E Prabhu; Yu, Wenbo; Fang, Lei; Alasady, Milad; Pierce, Adam D; Wilder, Paul T; MacKerell, Alexander D; Weber, David J

    2016-06-01

    Structure-based drug discovery is under way to identify and develop small-molecule S100B inhibitors (SBiXs). Such inhibitors have therapeutic potential for treating malignant melanoma, since high levels of S100B downregulate wild-type p53 tumor suppressor function in this cancer. Computational and X-ray crystallographic studies of two S100B-SBiX complexes are described, and both compounds (apomorphine hydrochloride and ethidium bromide) occupy an area of the S100B hydrophobic cleft which is termed site 3. These data also reveal novel protein-inhibitor interactions which can be used in future drug-design studies to improve SBiX affinity and specificity. Of particular interest, apomorphine hydrochloride showed S100B-dependent killing in melanoma cell assays, although the efficacy exceeds its affinity for S100B and implicates possible off-target contributions. Because there are no structural data available for compounds occupying site 3 alone, these studies contribute towards the structure-based approach to targeting S100B by including interactions with residues in site 3 of S100B. PMID:27303795

  10. Fourier-transform Ghost Imaging with Hard X-rays

    OpenAIRE

    Hong YU; Lu, Ronghua; Han, Shensheng; Xie, Honglan; Du, Guohao; Xiao, Tiqiao; Zhu, Daming

    2016-01-01

    Knowledge gained through X-ray crystallography fostered structural determination of materials and greatly facilitated the development of modern science and technology in the past century. Atomic details of sample structures is achievable by X-ray crystallography, however, it is only applied to crystalline structures. Imaging techniques based on X-ray coherent diffraction or zone plates are capable of resolving the internal structure of non-crystalline materials at nanoscales, but it is still ...

  11. High-resolution neutron and X-ray diffraction room-temperature studies of an H-FABP–oleic acid complex: study of the internal water cluster and ligand binding by a transferred multipolar electron-density distribution

    Directory of Open Access Journals (Sweden)

    E. I. Howard

    2016-03-01

    Full Text Available Crystal diffraction data of heart fatty acid binding protein (H-FABP in complex with oleic acid were measured at room temperature with high-resolution X-ray and neutron protein crystallography (0.98 and 1.90 Å resolution, respectively. These data provided very detailed information about the cluster of water molecules and the bound oleic acid in the H-FABP large internal cavity. The jointly refined X-ray/neutron structure of H-FABP was complemented by a transferred multipolar electron-density distribution using the parameters of the ELMAMII library. The resulting electron density allowed a precise determination of the electrostatic potential in the fatty acid (FA binding pocket. Bader's quantum theory of atoms in molecules was then used to study interactions involving the internal water molecules, the FA and the protein. This approach showed H...H contacts of the FA with highly conserved hydrophobic residues known to play a role in the stabilization of long-chain FAs in the binding cavity. The determination of water hydrogen (deuterium positions allowed the analysis of the orientation and electrostatic properties of the water molecules in the very ordered cluster. As a result, a significant alignment of the permanent dipoles of the water molecules with the protein electrostatic field was observed. This can be related to the dielectric properties of hydration layers around proteins, where the shielding of electrostatic interactions depends directly on the rotational degrees of freedom of the water molecules in the interface.

  12. Crystal growth and preliminary X-ray study of glutamic acid specific serine protease from Bacillus intermedius

    Science.gov (United States)

    Kuranova, I. P.; Blagova, E. V.; Levdikov, V. M.; Rudenskaya, G. N.; Balaban, N. P.; Shakirov, E. V.

    1999-01-01

    The glutamic acid specific protease (glutamyl-endopeptidase) from Bacillus intermedius, strain 3-19, was isolated and purified using ion exchange chromatography on CM-cellulose and Mono-S FPLC column. The conditions for crystallization of the enzyme have been discussed. The crystals of enzyme were grown using hanging-drop vapor-diffusion technique. Crystals belong to the space group C2 with unit cell parameters of a=61.62 Å, b=55.84 Å, c=60.40 Å, β=117.6° X-ray diffraction data to 1.68 Å resolution were collected using synchrotron radiation (EMBL, Hamburg) and an imaging plate scanner.

  13. Structure of HI-6*sarin-acetylcholinesterase determined by X-ray crystallography and molecular dynamics simulation: reactivator mechanism and design.

    Directory of Open Access Journals (Sweden)

    Fredrik Ekström

    Full Text Available Organophosphonates such as isopropyl metylphosphonofluoridate (sarin are extremely toxic as they phosphonylate the catalytic serine residue of acetylcholinesterase (AChE, an enzyme essential to humans and other species. Design of effective AChE reactivators as antidotes to various organophosphonates requires information on how the reactivators interact with the phosphonylated AChEs. However, such information has not been available hitherto because of three main challenges. First, reactivators are generally flexible in order to change from the ground state to the transition state for reactivation; this flexibility discourages determination of crystal structures of AChE in complex with effective reactivators that are intrinsically disordered. Second, reactivation occurs upon binding of a reactivator to the phosphonylated AChE. Third, the phosphorous conjugate can develop resistance to reactivation. We have identified crystallographic conditions that led to the determination of a crystal structure of the sarin(nonaged-conjugated mouse AChE in complex with [(E-[1-[(4-carbamoylpyridin-1-ium-1-ylmethoxymethyl]pyridin-2-ylidene]methyl]-oxoazanium dichloride (HI-6 at a resolution of 2.2 A. In this structure, the carboxyamino-pyridinium ring of HI-6 is sandwiched by Tyr124 and Trp286, however, the oxime-pyridinium ring is disordered. By combining crystallography with microsecond molecular dynamics simulation, we determined the oxime-pyridinium ring structure, which shows that the oxime group of HI-6 can form a hydrogen-bond network to the sarin isopropyl ether oxygen, and a water molecule is able to form a hydrogen bond to the catalytic histidine residue and subsequently deprotonates the oxime for reactivation. These results offer insights into the reactivation mechanism of HI-6 and design of better reactivators.

  14. X-ray investigation of gene-engineered human insulin crystallized from a solution containing polysialic acid

    International Nuclear Information System (INIS)

    Crystals of insulin have been grown from a solution containing insulin and polysialic acid and the three-dimensional structure of insulin in these crystals has been solved at 1.6 Å resolution. Attempts to crystallize the noncovalent complex of recombinant human insulin with polysialic acid were carried out under normal and microgravity conditions. Both crystal types belonged to the same space group, I213, with unit-cell parameters a = b = c = 77.365 Å, α = β = γ = 90.00°. The reported space group and unit-cell parameters are almost identical to those of cubic insulin reported in the PDB. The results of X-ray studies confirmed that the crystals obtained were cubic insulin crystals and that they contained no polysialic acid or its fragments. Electron-density maps were calculated using X-ray diffraction sets from earth-grown and microgravity-grown crystals and the three-dimensional structure of the insulin molecule was determined and refined. The conformation and secondary-structural elements of the insulin molecule in different crystal forms were compared

  15. Synthesis and X-ray Crystallography of [Mg(H2O)6][AnO2(C2H5COO)3]2 (An = U, Np, or Pu).

    Science.gov (United States)

    Serezhkin, Viktor N; Grigoriev, Mikhail S; Abdulmyanov, Aleksey R; Fedoseev, Aleksandr M; Savchenkov, Anton V; Serezhkina, Larisa B

    2016-08-01

    Synthesis and X-ray crystallography of single crystals of [Mg(H2O)6][AnO2(C2H5COO)3]2, where An = U (I), Np (II), or Pu (III), are reported. Compounds I-III are isostructural and crystallize in the trigonal crystal system. The structures of I-III are built of hydrated magnesium cations [Mg(H2O)6](2+) and mononuclear [AnO2(C2H5COO)3](-) complexes, which belong to the AB(01)3 crystallochemical group of uranyl complexes (A = AnO2(2+), B(01) = C2H5COO(-)). Peculiarities of intermolecular interactions in the structures of [Mg(H2O)6][UO2(L)3]2 complexes depending on the carboxylate ion L (acetate, propionate, or n-butyrate) are investigated using the method of molecular Voronoi-Dirichlet polyhedra. Actinide contraction in the series of U(VI)-Np(VI)-Pu(VI) in compounds I-III is reflected in a decrease in the mean An═O bond lengths and in the volume and sphericity degree of Voronoi-Dirichlet polyhedra of An atoms. PMID:27404584

  16. Particle-induced x-ray emission: Instrumentation, calibration, and application to contact lens solutions and fulvic acid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Jenson, D.D.

    1989-01-01

    An expression was derived describing the profile of the proton beam at the PIXE target position. The expression was used to predict the profile for several experimental configurations. The profile was experimentally measured. The PIXE system was calibrated using solutions and commercial foils. Experimental data was adjusted for all absorbers and interferences, and a quadratic relationship was determined relating calibration factor and atomic number for each series of X-ray transitions. Calibration factors were determined for all elements above aluminum, for both a pinhole filter and a 14-mil mylar filter. A group of contact lens solutions was analyzed using PIXE, ICP, and ISE. A digestion method was developed for removal. of chloride ion. Cluster analysis was used to classify the data. A commercial humic acid was separated into three fractions. The fulvic acid was characterized, and separations of metal-fulvic acid complexes from metal ions in solution were attempted using ultrafiltration.

  17. Understanding nucleic acid structural changes by comparing wide-angle x-ray scattering (WAXS) experiments to molecular dynamics simulations

    Science.gov (United States)

    Pabit, Suzette A.; Katz, Andrea M.; Tolokh, Igor S.; Drozdetski, Aleksander; Baker, Nathan; Onufriev, Alexey V.; Pollack, Lois

    2016-05-01

    Wide-angle x-ray scattering (WAXS) is emerging as a powerful tool for increasing the resolution of solution structure measurements of biomolecules. Compared to its better known complement, small angle x-ray scattering (SAXS), WAXS targets higher scattering angles and can enhance structural studies of molecules by accessing finer details of solution structures. Although the extension from SAXS to WAXS is easy to implement experimentally, the computational tools required to fully harness the power of WAXS are still under development. Currently, WAXS is employed to study structural changes and ligand binding in proteins; however, the methods are not as fully developed for nucleic acids. Here, we show how WAXS can qualitatively characterize nucleic acid structures as well as the small but significant structural changes driven by the addition of multivalent ions. We show the potential of WAXS to test all-atom molecular dynamics (MD) simulations and to provide insight into understanding how the trivalent ion cobalt(III) hexammine (CoHex) affects the structure of RNA and DNA helices. We find that MD simulations capture the RNA structural change that occurs due to addition of CoHex.

  18. Crystallization and X-ray diffraction studies of a complete bacterial fatty-acid synthase type I

    Energy Technology Data Exchange (ETDEWEB)

    Enderle, Mathias [Goethe University Frankfurt, Max-von-Laue-Strasse 15, 60438 Frankfurt am Main (Germany); Max-Planck-Institute of Biochemistry, Am Klopferspitz 18, 82152 Martinsried (Germany); McCarthy, Andrew [EMBL Grenoble, 71 Avenue des Martyrs, 38042 Grenoble CEDEX 9 (France); Paithankar, Karthik Shivaji, E-mail: paithankar@em.uni-frankfurt.de [Goethe University Frankfurt, Max-von-Laue-Strasse 15, 60438 Frankfurt am Main (Germany); Grininger, Martin, E-mail: paithankar@em.uni-frankfurt.de [Goethe University Frankfurt, Max-von-Laue-Strasse 15, 60438 Frankfurt am Main (Germany); Max-Planck-Institute of Biochemistry, Am Klopferspitz 18, 82152 Martinsried (Germany)

    2015-10-23

    Bacterial and fungal type I fatty-acid synthases (FAS I) are evolutionarily connected, as bacterial FAS I is considered to be the ancestor of fungal FAS I. In this work, the production, crystallization and X-ray diffraction data analysis of a bacterial FAS I are reported. While a deep understanding of the fungal and mammalian multi-enzyme type I fatty-acid synthases (FAS I) has been achieved in recent years, the bacterial FAS I family, which is narrowly distributed within the Actinomycetales genera Mycobacterium, Corynebacterium and Nocardia, is still poorly understood. This is of particular relevance for two reasons: (i) although homologous to fungal FAS I, cryo-electron microscopic studies have shown that bacterial FAS I has unique structural and functional properties, and (ii) M. tuberculosis FAS I is a drug target for the therapeutic treatment of tuberculosis (TB) and therefore is of extraordinary importance as a drug target. Crystals of FAS I from C. efficiens, a homologue of M. tuberculosis FAS I, were produced and diffracted X-rays to about 4.5 Å resolution.

  19. Understanding Nucleic Acid Structural Changes by Comparing Wide-Angle X-ray Scattering (WAXS) Experiments to Molecular Dynamics Simulations

    Energy Technology Data Exchange (ETDEWEB)

    Pabit, Suzette; Katz, Andrea M.; Tolokh, Igor S.; Drozdetski, Aleksander; Baker, Nathan A.; Onufriev, Alexey; Pollack, Lois

    2016-05-24

    Wide-angle x-ray scattering (WAXS) is emerging as a powerful tool for increasing the resolution of solution structure measurements of biomolecules. Compared to its better known complement, small angle x-ray scattering (SAXS), WAXS targets higher scattering angles and can enhance structural studies of molecules by accessing finer details of solution structures. Although the extension from SAXS to WAXS is easy to implement experimentally, the computational tools required to fully harness the power of WAXS are still under development. Currently, WAXS is employed to study structural changes and ligand binding in proteins; however the methods are not as fully developed for nucleic acids. Here, we show how WAXS can qualitatively char- acterize nucleic acid structures as well as the small but significant structural changes driven by the addition of multivalent ions. We show the potential of WAXS to test all-atom molecular dynamics (MD) simulations and to provide insight in understanding how the trivalent ion cobalt(III) hexammine (CoHex) affects the structure of RNA and DNA helices. We find that MD simulations capture the RNA structural change that occurs due to addition of CoHex.

  20. Fast and simple method for determination of fatty acid methyl esters (FAME) in biodiesel blends using X-ray spectrometry.

    Science.gov (United States)

    Sitko, Rafal; Zawisza, Beata; Kowalewska, Zofia; Kocot, Karina; Polowniak, Marzena

    2011-09-30

    The determination of fatty acid methyl esters (FAME) in diesel fuel blends is an important aspect of production and blending process as well as quality control of distribution operations. In this study, energy-dispersive X-ray fluorescence spectrometer (EDXRF) is used for the first time for determination of FAME in biodiesel blends. The principle of the method is based on intensity difference of X-ray radiation scattered from hydrocarbons and from FAME. The experiment shows that coherent and incoherent radiation, commonly applied for evaluation of the average atomic number of the sample with light matrix, cannot be applied for FAME determination. However, the application of scattered continuous radiation gives excellent correlation between FAME concentration and intensity of scattered radiation. The best results are obtained if continuum is collected in the range of energy between 10.5 and 15.0 keV for rhodium X-ray tube, operated at 35 kV. Linear relationship between the FAME concentration and the inverse of scattered continuous radiation is obtained with the correlation coefficients of 0.999. Standard deviation of measurement is ca. 0.46% (v/v) of FAME and detection limit is 1.2% (v/v) for 600 s counting time and 50% dead-time loss using Si-PIN detector. The investigation shows that crucial issue in determination of FAME in biodiesel blends using EDXRF spectrometer is the precision of measurements resulting from the counting statistics. Therefore, much better results (0.20% (v/v) standard deviation and 0.52% (v/v) detection limit) can be expected if higher intensity of primary radiation is applied and X-ray spectrum is collected by silicon drift detector of high input count rate. For concentration of FAME from 10 to 100% (v/v), the differences between reference method (Fourier transform infrared spectrometry) and the proposed method usually do not exceed 1% (v/v) of FAME. The proposed method is fast, simple and enables FAME determination in wide range of

  1. X-Rays

    Science.gov (United States)

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat ...

  2. Acid-beta-glycerophosphatase reaction products in the central nervous system mitochondria following x-ray irradiation.

    Science.gov (United States)

    Roizin, L; Orlovskaja, D; Liu, J C; Carsten, A L

    1975-06-01

    A survey of the literature to date on the enzyme histochemistry of intracellular organelles has not yielded any reference to the presence of acid phosphatase reaction products in the mammalian mitochondria of the central nervous system. A combination of Gomori's acid phosphatase mehtod, however, with standard electron microscopy has disclosed the presence of enzyme reaction products in the mitochondria of the central nervous system of rats from 2 hr to 22 weeks after x-ray irradiation, as well as in a cerebral biopsy performed on a patient affected by Huntington's chorea. No enzyme reaction products, on the other hand, were observed in serial sections that had been incubated in substrates either containing sodium fluoride or lacking in beta-glycerophosphate. The abnormal mitochondrial enzyme reaction (chemical lesion) is considered to be the consequenco of the pathologic process affecting the ultrastructural-chemical organization of the organelle.

  3. Acid-β-glycerophosphatase reaction products in the central nervous system mitochondria following x-ray irradiation

    International Nuclear Information System (INIS)

    A survey of the literature to date on the enzyme histochemistry of intracellular organelles has not yielded any reference to the presence of acid phosphatase reaction products in the mammalian mitochondria of the central nervous system. A combination of Gomori's acid phosphatase method, however, with standard electron microscopy has disclosed the presence of enzyme reaction products in the mitochondria of the central nervous system of rats from 2 hr to 22 weeks after x-ray irradiation, as well as in a cerebral biopsy performed on a patient affected by Huntington's chorea. No enzyme reaction products, on the other hand, were observed in serial sections that had been incubated in substrates either containing sodium fluoride or lacking in β-glycerophosphate. The abnormal mitochondrial enzyme reaction (chemical lesion) is considered to be the consequence of the pathologic process affecting the ultrastructural-chemical organization of the organelle

  4. X-ray diffraction

    International Nuclear Information System (INIS)

    We have been interested in structural elucidation by x-ray diffraction of compounds of biological interest. Understanding exactly how atoms are arranged in three-dimensional arrays as molecules can help explain the relationship between structure and functions. The species investigated may vary in size and shape; our recent studies included such diverse substances as antischistosomal drugs, a complex of cadmium with nucleic acid base, nitrate salts of adenine, and proteins

  5. Speciation of sulfur in humic and fulvic acids using X-ray absorption near-edge structure (XANES) spectroscopy

    Science.gov (United States)

    Morra, Matthew J.; Fendorf, Scott E.; Brown, Paul D.

    1997-02-01

    Sulfur species in soils and sediments have previously been determined indirectly using destructive techniques. A direct and more accurate method for S speciation would improve our understanding of S biogeochemistry. X-ray absorption near edge structure (XANES) spectroscopy was performed on purified humic and fulvic acids from terrestrial and aquatic environments. This methodology allows direct determination of S species using the relationship that exists with the energy required for core electron transitions and in some cases, correlation with additional spectral features. Soil, peat, and aquatic humic acids were dominated by sulfonates with an oxidation state of +5, but also contained ester-bonded sulfates with an oxidation state of +6. Leonardite humic acid contained ester-bonded sulfate and an unidentified S compound with an oxidation state of +4.0. In contrast, high-valent S in soil, peat, and aquatic fulvic acids was exclusively in the form of sulfonic acids. Reduced S species were also present in both humic and fulvic acids. XANES is a valuable method for the speciation of S in humic materials and of potential use in S speciation of unfractionated soils.

  6. Speciation of sulfur in humic and fulvic acids using X-ray Absorption Near-Edge Structures (XANES) spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Morra, M.J.; Fendorf, S.E.; Brown, P.D. [Univ. of Idaho, Moscow, ID (United States)

    1997-02-01

    Sulfur species in soils and sediments have previously been determined indirectly using destructive techniques. A direct and more accurate method for S speciation would improve our understanding of S biogeochemistry. X-ray absorption near edge structure (XANES) spectroscopy was performed on purified humic and fulvic acids from terrestrial and aquatic environments. This methodology allows direct determination of S species using the relationship that exists with the energy required for core electron transitions and in some cases, correlation with additional spectral features. Soil, peat, and aquatic humic acids were dominated by sulfonates with an oxidation state of +5, but also contained ester-bonded sulfates with an oxidation state of +6. Leonardite humic acid contained ester-bonded sulfate and an unidentified S compound with an oxidation state of +4.0. In contrast, high-valent S in soil, peat, and aquatic fulvic acids was exclusively in the form of sulfonic acids. Reduced S species were also present in both humic and fulvic acids. XANES is a valuable method for the speciation of S in humic materials and of potential use in S speciation of unfractionated soils. 27 refs., 4 figs., 3 tabs.

  7. An X-ray photoelectron spectroscopy study of the acidity of SiO{sub 2}-ZrO{sub 2} mixed oxides

    Energy Technology Data Exchange (ETDEWEB)

    Bosman, H.J.M.; Pijpers, A.P.; Jaspers, A.W.M.A. [DSM Research B.V., MD Geleen (Netherlands)

    1996-07-01

    X-ray photoelectron spectroscopy (XPS) of SiO{sub 2}-ZrO{sub 2} mixed oxides was studied. Surface acidity was investigated in light of the relationship between acidity and catalytic effects. 28 refs., 12 figs., 3 tabs.

  8. Chest x-ray

    Science.gov (United States)

    Chest radiography; Serial chest x-ray; X-ray - chest ... You stand in front of the x-ray machine. You will be told to hold your breath when the x-ray is taken. Two images are usually taken. You will ...

  9. X-Ray Characterisation of Various Aluminium Phases in the Medicinal Herb Bacopa Monnieri Affected by Simulated Acid Rain

    Directory of Open Access Journals (Sweden)

    B. Mallick

    2012-07-01

    Full Text Available In the present investigation various aluminium-based new phases formed due to substitution of sulphur via simulated acid rain in Bacopa monnieri have been analyzed using X-ray diffraction (XRD technique. So far there is no report on the effects of acid rain on the B. monnieri herb and its vital properties like memory-boosting mechanism. Therefore, in the present study, an attempt has been made to analyze the various aluminium phase (salt formations due to the substitution of sulphur via simulated acid rain (SiAR in B. Monnieri because of its toxicological importance. The new phases like AlH(SO42 and Al2S3 along with usual Al2O3:H2O, MgO, FeAl2(PO42(OH2:8H2O, (K2Ca(SO42:H2O, have been observed in B. monnieri when treated with sulphuric-simulated acid rain (S-SiAR of two different pH (3.39 and 5.45 for 20 weeks. These Al-based new salts formed in the above medicinal herb due to the induction of S-SiAR may cause Alzheimer’s disease and induce other abnormities.

  10. Accurate small and wide angle x-ray scattering profiles from atomic models of proteins and nucleic acids

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, Hung T. [BioMaPS Institute for Quantitative Biology, Rutgers University, Piscataway, New Jersey 08854 (United States); Pabit, Suzette A.; Meisburger, Steve P.; Pollack, Lois [School of Applied and Engineering Physics, Cornell University, Ithaca, New York 14853 (United States); Case, David A., E-mail: case@biomaps.rutgers.edu [BioMaPS Institute for Quantitative Biology, Rutgers University, Piscataway, New Jersey 08854 (United States); Department of Chemistry and Chemical Biology, Rutgers University, Piscataway, New Jersey 08854 (United States)

    2014-12-14

    A new method is introduced to compute X-ray solution scattering profiles from atomic models of macromolecules. The three-dimensional version of the Reference Interaction Site Model (RISM) from liquid-state statistical mechanics is employed to compute the solvent distribution around the solute, including both water and ions. X-ray scattering profiles are computed from this distribution together with the solute geometry. We describe an efficient procedure for performing this calculation employing a Lebedev grid for the angular averaging. The intensity profiles (which involve no adjustable parameters) match experiment and molecular dynamics simulations up to wide angle for two proteins (lysozyme and myoglobin) in water, as well as the small-angle profiles for a dozen biomolecules taken from the BioIsis.net database. The RISM model is especially well-suited for studies of nucleic acids in salt solution. Use of fiber-diffraction models for the structure of duplex DNA in solution yields close agreement with the observed scattering profiles in both the small and wide angle scattering (SAXS and WAXS) regimes. In addition, computed profiles of anomalous SAXS signals (for Rb{sup +} and Sr{sup 2+}) emphasize the ionic contribution to scattering and are in reasonable agreement with experiment. In cases where an absolute calibration of the experimental data at q = 0 is available, one can extract a count of the excess number of waters and ions; computed values depend on the closure that is assumed in the solution of the Ornstein–Zernike equations, with results from the Kovalenko–Hirata closure being closest to experiment for the cases studied here.

  11. Rigid body essential X-ray crystallography

    DEFF Research Database (Denmark)

    Bjerrum, Esben Jannik; Biggin, Philip C

    2008-01-01

    The ligand-binding domain (LBD) from the ionotropic glutamate receptor subtype 2 (GluR2) has been shown to adopt a range of ligand-dependent conformational states. These states have been described in terms of the rotation required to fit subdomain (lobe) 2 following superposition of subdomain (lo...

  12. [Computed X-ray tomography in predicting the efficacy of oral cholelithiasis with bile acids].

    Science.gov (United States)

    Fu, X B

    1993-02-01

    The efficacy of oral cholelitholytic therapy with chenodeoxycholic acid (CDCA) and ursodeoxycholic acid (UDCA) in 137 patients with gallstones was compared with their CT patterns. The best dissolving results were obtained from patients with the stones in isodense and faint category (OCG). Besides, gallstones, which showed no obvious filling defect on OCG but distinct echo and shadow on B-type ultrasonography, were also insoluble. PMID:8391902

  13. Conjugated linoleic acid inhibiting DNA repair damaged by x-ray

    International Nuclear Information System (INIS)

    Non-homologous end-joining is the most effective repair of DNA double strand break. Epidermal growth factor receptor activates DSB repairs. Integration of EGFR inhibitors with radiation or chemotherapy were used in lung cancer treatment. Radiosensitivity effect of conjugated linoleic acid on tumor cells and reduced metastasis are reported

  14. Isolation and x-ray structure of deoxycholic acid from the sponge Ircinia sp.

    Digital Repository Service at National Institute of Oceanography (India)

    Singh, K.S.; Kaminsky, W.

    Ethyl acetate extract of the sponge Ircinia sp., collected by SCUBA divers off the coast of southern India, contained a cholest-based sterol of insignificant antimicrobial activity, with one carboxylic acid side chain (3 Alpha, 7 Beta-dihydroxy-5...

  15. Thoracic spine x-ray

    Science.gov (United States)

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... care provider's office. You will lie on the x-ray table in different positions. If the x-ray ...

  16. X-ray (image)

    Science.gov (United States)

    X-rays are a form of ionizing radiation that can penetrate the body to form an image on ... will be shades of gray depending on density. X-rays can provide information about obstructions, tumors, and other ...

  17. Dental x-rays

    Science.gov (United States)

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film ... dentist's office. There are many types of dental x-rays. Some are: Bitewing Periapical Palatal (also called occlusal) ...

  18. X-ray apparatus

    International Nuclear Information System (INIS)

    A diagnostic x-ray device, readily convertible between conventional radiographic and tomographic operating modes, is described. An improved drive system interconnects and drives the x-ray source and the imaging device through coordinated movements for tomography

  19. Dental x-rays

    Science.gov (United States)

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film; Digital image ... dentist's office. There are many types of dental x-rays. Some of them are: Bitewing. Shows the crown ...

  20. X-ray crystallographic studies of metalloproteins.

    Science.gov (United States)

    Volbeda, Anne

    2014-01-01

    Many proteins require metals for their physiological function. In combination with spectroscopic characterizations, X-ray crystallography is a very powerful method to correlate the function of protein-bound metal sites with their structure. Due to their special X-ray scattering properties, specific metals may be located in metalloprotein structures and eventually used for phasing the diffracted X-rays by the method of Multi-wavelength Anomalous Dispersion (MAD). How this is done is the principle subject of this chapter. Attention is also given to the crystallographic characterization of different oxidation states of redox active metals and to the complication of structural changes that may be induced by X-ray irradiation of protein crystals.

  1. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    CERN Document Server

    Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

  2. X-Rays

    Science.gov (United States)

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of your ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat and ...

  3. Chest X-Ray

    Medline Plus

    Full Text Available ... by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, ... you about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed ...

  4. X-Ray Imaging

    Science.gov (United States)

    ... Brain Surgery Imaging Clinical Trials Basics Patient Information X-Ray Imaging Print This Page X-ray imaging is perhaps the most familiar type of imaging. Images produced by X-rays are due to the different absorption rates of ...

  5. Bioabsorbable bone fixation plates for X-ray imaging diagnosis by a radiopaque layer of barium sulfate and poly(lactic-co-glycolic acid).

    Science.gov (United States)

    Choi, Sung Yoon; Hur, Woojune; Kim, Byeung Kyu; Shasteen, Catherine; Kim, Myung Hun; Choi, La Mee; Lee, Seung Ho; Park, Chun Gwon; Park, Min; Min, Hye Sook; Kim, Sukwha; Choi, Tae Hyun; Choy, Young Bin

    2015-04-01

    Bone fixation systems made of biodegradable polymers are radiolucent, making post-operative diagnosis with X-ray imaging a challenge. In this study, to allow X-ray visibility, we separately prepared a radiopaque layer and attached it to a bioabsorbable bone plate approved for clinical use (Inion, Finland). We employed barium sulfate as a radiopaque material due to the high X-ray attenuation coefficient of barium (2.196 cm(2) /g). The radiopaque layer was composed of a fine powder of barium sulfate bound to a biodegradable material, poly(lactic-co-glycolic acid) (PLGA), to allow layer degradation similar to the original Inion bone plate. In this study, we varied the mass ratio of barium sulfate and PLGA in the layer between 3:1 w/w and 10:1 w/w to modulate the degree and longevity of X-ray visibility. All radiopaque plates herein were visible via X-ray, both in vitro and in vivo, for up to 40 days. For all layer types, the radio-opacity decreased with time due to the swelling and degradation of PLGA, and the change in the layer shape was more apparent for layers with a higher PLGA content. The radiopaque plates released, at most, 0.5 mg of barium sulfate every 2 days in a simulated in vitro environment, which did not appear to affect the cytotoxicity. The radiopaque plates also exhibited good biocompatibility, similar to that of the Inion plate. Therefore, we concluded that the barium sulfate-based, biodegradable plate prepared in this work has the potential to be used as a fixation device with both X-ray visibility and biocompatibility.

  6. X-ray absorption and resonance raman spectroscopy of human myeloperoxidase at neutral and acid pH.

    Science.gov (United States)

    Yue, K T; Taylor, K L; Kinkade, J M; Sinclair, R B; Powers, L S

    1997-04-01

    Myeloperoxidase (MPO), an important enzyme in the oxygen-dependent host defense system of human polymorphonuclear leukocytes, utilizes hydrogen peroxide to catalyze the production of hypochlorous acid, an oxidizing bactericidal agent. While MPO shows significant sequence homology with other peroxidases and this homology is particularly striking among the active-site residues, MPO exhibits unusual spectral features and the unique ability to catalyze the oxidation of chloride ions. We have investigated the MPO active-site with X-ray absorption (XAS) and resonance Raman (RRS) spectroscopies at neutral pH and also at the physiological acidic pH (pH approximately 3) and have compared these results with those of horseradish peroxidase (HRP). At pH 7.5, XAS results show that the iron heme active site is 6-coordinate where the distal ligand is likely nitrogen or oxygen, but not sulfur. The heme is distorted compared to HRP, other peroxidases, and heme compounds, but at pH approximately 3, the distal ligand is lost and the heme is less distorted. RRS results under identical pH conditions show that the skeletal core-size sensitive modes and v3 are shifted to higher frequency at pH approximately 3 indicating a 6- to 5-coordination change of high spin ferric heme. In addition, a new band at 270 cm(-1) is observed at pH approximately 3 which is consistent with the loss of the sixth ligand. The higher symmetry of the heme at pH approximately 3 is reflected by a single v4 mode in the (RRS) spectrum. HRP also loses its loosely associated distal water at this pH, but little change in heme distortion is observed. This change suggests that loss of the distal ligand in MPO releases stress on the heme which may facilitate binding of chloride ion.

  7. Crystallization and preliminary X-ray diffraction analysis of the sialic acid-binding domain (VP8*) of porcine rotavirus strain CRW-8

    Energy Technology Data Exchange (ETDEWEB)

    Scott, Stacy A. [Institute for Glycomics, Griffith University (Gold Coast Campus) PMB 50, Gold Coast Mail Centre, Queensland 9726 (Australia); Holloway, Gavan; Coulson, Barbara S. [Department of Microbiology and Immunology, The University of Melbourne, Victoria 3010 (Australia); Szyczew, Alex J.; Kiefel, Milton J.; Itzstein, Mark von; Blanchard, Helen, E-mail: h.blanchard@griffith.edu.au [Institute for Glycomics, Griffith University (Gold Coast Campus) PMB 50, Gold Coast Mail Centre, Queensland 9726 (Australia)

    2005-06-01

    The sialic acid-binding domain (VP8*) component of the porcine CRW-8 rotavirus spike protein has been overexpressed in E. coli, purified and co-crystallized with an N-acetylneuraminic acid derivative. X-ray diffraction data have been collected to 2.3 Å, which has enabled determination of the structure by molecular replacement. Rotavirus recognition and attachment to host cells involves interaction with the spike protein VP4 that projects outwards from the surface of the virus particle. An integral component of these spikes is the VP8* domain, which is implicated in the direct recognition and binding of sialic acid-containing cell-surface carbohydrates and facilitates subsequent invasion by the virus. The expression, purification, crystallization and preliminary X-ray diffraction analysis of VP8* from porcine CRW-8 rotavirus is reported. Diffraction data have been collected to 2.3 Å resolution, enabling the determination of the VP8* structure by molecular replacement.

  8. Polyglycolic acid-polylactic acid scaffold response to different progenitor cell in vitro cultures: a demonstrative and comparative X-ray synchrotron radiation phase-contrast microtomography study.

    Science.gov (United States)

    Giuliani, Alessandra; Moroncini, Francesca; Mazzoni, Serena; Belicchi, Marzia Laura Chiara; Villa, Chiara; Erratico, Silvia; Colombo, Elena; Calcaterra, Francesca; Brambilla, Lucia; Torrente, Yvan; Albertini, Gianni; Della Bella, Silvia

    2014-04-01

    Spatiotemporal interactions play important roles in tissue development and function, especially in stem cell-seeded bioscaffolds. Cells interact with the surface of bioscaffold polymers and influence material-driven control of cell differentiation. In vitro cultures of different human progenitor cells, that is, endothelial colony-forming cells (ECFCs) from a healthy control and a patient with Kaposi sarcoma (an angioproliferative disease) and human CD133+ muscle-derived stem cells (MSH 133+ cells), were seeded onto polyglycolic acid-polylactic acid scaffolds. Three-dimensional (3D) images were obtained by X-ray phase-contrast microtomography (micro-CT) and processed with the Modified Bronnikov Algorithm. The method enabled high spatial resolution detection of the 3D structural organization of cells on the bioscaffold and evaluation of the way and rate at which cells modified the construct at different time points from seeding. The different cell types displayed significant differences in the proliferation rate. In conclusion, X-ray synchrotron radiation phase-contrast micro-CT analysis proved to be a useful and sensitive tool to investigate the spatiotemporal pattern of progenitor cell organization on a bioscaffold.

  9. The role of the arachidonic acid cascade in the species-specific X-ray-induced inflammation of the rabbit eye

    Energy Technology Data Exchange (ETDEWEB)

    Bito, L.Z.; Klein, E.M.

    1982-05-01

    To identify the mediator(s) of the apparently species-specific X-ray-induced inflammation of the rabbit eye, inhibitors of the synthesis and/or release of known or putative mediators of ocular inflammation were administered prior to irradiation. The X-ray-induced ocular inflammation, particularly the rise in intraocular pressure, was found to be inhibited by intravenous pretreatment of rabbits with flurbiprofen, indomethacin, or imidazole (1, 10, and 100 mg/kg i.v., respectively), or by combined intravitreal and topical administration of flurbiprofen. Systemic, intravitreal, and/or topical pretreatment with prednisolone or disodium cromoglycate or the retrobulbar injection of ethyl alcohol or capsaicin failed to block the inflammatory response, whereas vitamin E apparently exerted some protective effect. These findings show that the X-ray-induced inflammation of the rabbit eye is mediated, at least in part, by prostaglandins (PGs) and/or related autacoids. In addition, these results suggest that the unique sensitivity of the rabbit eye to X-ray-induced inflammation is due either to the presence in this species of a unique or uniquely effective triggering mechanism for the release of PG precursors or to the greater sensitivity of this species to the ocular inflammatory effects of PGs. Thus the rabbit eye may provide a unique model for studying some aspects of arachidonic acid release or ocular PG effects, but extreme caution must be exercised in generalizing such findings to other species.

  10. Preconcentration of submicrogram amounts of metals from natural water for X-ray energy spectrometric determination using pyrrolidinecarbodithioic acid

    International Nuclear Information System (INIS)

    A method was developed for the routine determination of several trace metals in natural waters by X-ray energy spectrometry following precipitation with pyrrolidinecarbodithioate. Preoxidation with persulfate eliminates interferences by organic matter. By optimizing carrier ion selection and measurement conditions, one may determine dithioate-reactive elements with Z less than or equal to 50 by means of their K X-rays, and some with Z greater than or equal to 80 by means of their L X-rays. Determinations are feasible for several elements at concentrations down to 250 ng L-1, or below. Recoveries are generally greater than 90%, although some exceptions are noted. Reproducibility with real samples averaged about 25% relative standard deviation for five representative elements at concentrations above 250 ng L-1. 24 references, 5 figures, 4 tables

  11. The future of crystallography in drug discovery

    Science.gov (United States)

    Zheng, Heping; Hou, Jing; Zimmerman, Matthew D; Wlodawer, Alexander; Minor, Wladek

    2014-01-01

    Introduction X-ray crystallography plays an important role in structure-based drug design (SBDD), and accurate analysis of crystal structures of target macromolecules and macromolecule–ligand complexes is critical at all stages. However, whereas there has been significant progress in improving methods of structural biology, particularly in X-ray crystallography, corresponding progress in the development of computational methods (such as in silico high-throughput screening) is still on the horizon. Crystal structures can be overinterpreted and thus bias hypotheses and follow-up experiments. As in any experimental science, the models of macromolecular structures derived from X-ray diffraction data have their limitations, which need to be critically evaluated and well understood for structure-based drug discovery. Areas covered This review describes how the validity, accuracy and precision of a protein or nucleic acid structure determined by X-ray crystallography can be evaluated from three different perspectives: i) the nature of the diffraction experiment; ii) the interpretation of an electron density map; and iii) the interpretation of the structural model in terms of function and mechanism. The strategies to optimally exploit a macromolecular structure are also discussed in the context of ‘Big Data’ analysis, biochemical experimental design and structure-based drug discovery. Expert opinion Although X-ray crystallography is one of the most detailed ‘microscopes’ available today for examining macromolecular structures, the authors would like to re-emphasize that such structures are only simplified models of the target macromolecules. The authors also wish to reinforce the idea that a structure should not be thought of as a set of precise coordinates but rather as a framework for generating hypotheses to be explored. Numerous biochemical and biophysical experiments, including new diffraction experiments, can and should be performed to verify or falsify

  12. X-Ray Polarimetry

    CERN Document Server

    Kaaret, Philip

    2014-01-01

    We review the basic principles of X-ray polarimetry and current detector technologies based on the photoelectric effect, Bragg reflection, and Compton scattering. Recent technological advances in high-spatial-resolution gas-filled X-ray detectors have enabled efficient polarimeters exploiting the photoelectric effect that hold great scientific promise for X-ray polarimetry in the 2-10 keV band. Advances in the fabrication of multilayer optics have made feasible the construction of broad-band soft X-ray polarimeters based on Bragg reflection. Developments in scintillator and solid-state hard X-ray detectors facilitate construction of both modular, large area Compton scattering polarimeters and compact devices suitable for use with focusing X-ray telescopes.

  13. X-Ray Polarimetry

    OpenAIRE

    Kaaret, Philip

    2014-01-01

    We review the basic principles of X-ray polarimetry and current detector technologies based on the photoelectric effect, Bragg reflection, and Compton scattering. Recent technological advances in high-spatial-resolution gas-filled X-ray detectors have enabled efficient polarimeters exploiting the photoelectric effect that hold great scientific promise for X-ray polarimetry in the 2-10 keV band. Advances in the fabrication of multilayer optics have made feasible the construction of broad-band ...

  14. Liquid structure of acetic acid-water and trifluoroacetic acid-water mixtures studied by large-angle X-ray scattering and NMR.

    Science.gov (United States)

    Takamuku, Toshiyuki; Kyoshoin, Yasuhiro; Noguchi, Hiroshi; Kusano, Shoji; Yamaguchi, Toshio

    2007-08-01

    The structures of acetic acid (AA), trifluoroacetic acid (TFA), and their aqueous mixtures over the entire range of acid mole fraction xA have been investigated by using large-angle X-ray scattering (LAXS) and NMR techniques. The results from the LAXS experiments have shown that acetic acid molecules mainly form a chain structure via hydrogen bonding in the pure liquid. In acetic acid-water mixtures hydrogen bonds of acetic acid-water and water-water gradually increase with decreasing xA, while the chain structure of acetic acid molecules is moderately ruptured. Hydrogen bonds among water molecules are remarkably formed in acetic acid-water mixtures at xATFA molecules form not a chain structure but cyclic dimers through hydrogen bonding in the pure liquid. In TFA-water mixtures O...O hydrogen bonds among water molecules gradually increase when xA decreases, and hydrogen bonds among water molecules are significantly formed in the mixtures at xATFA molecules are considerably dissociated to hydrogen ions and trifluoroacetate in the mixtures. 1H, 13C, and 19F NMR chemical shifts of acetic acid and TFA molecules for acetic acid-water and TFA-water mixtures have indicated strong relationships between a structural change of the mixtures and the acid mole fraction. On the basis of both LAXS and NMR results, the structural changes of acetic acid-water and TFA-water mixtures with decreasing acid mole fraction and the effects of fluorination of the methyl group on the structure are discussed at the molecular level. PMID:17628099

  15. X-ray - skeleton

    Science.gov (United States)

    A skeletal x-ray is an imaging test used to look at the bones. It is used to detect fractures , tumors, or ... in the health care provider's office by an x-ray technologist. You will lie on a table or ...

  16. Extremity x-ray

    Science.gov (United States)

    An extremity x-ray is an image of the hands, wrist, feet, ankle, leg, thigh, forearm humerus or upper arm, hip, shoulder ... term "extremity" often refers to a human limb. X-rays are a form of radiation that passes through ...

  17. X-ray interferometers

    International Nuclear Information System (INIS)

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  18. Femtosecond X-ray protein nanocrystallography

    Energy Technology Data Exchange (ETDEWEB)

    Chapman, Henry N. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Univ. of Hamburg (Germany); Barty, Anton [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; White, Thomas A. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Aquila, Andrew [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Schulz, Joachim [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; DePonte, Daniel P. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Martin, Andrew V. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Coppola, Nicola [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Liang, Mengning [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Caleman, Carl [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Gumprecht, Lars [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Stern, Stephan [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Nass, Karol [Univ. of Hamburg (Germany); Fromme, Petra [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Hunter, Mark S. [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Grotjohann, Ingo [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Fromme, Raimund [Arizona State Univ., Tempe, AZ (United States). Dept. of Chemistry and Biochemistry; Kirian, Richard A. [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Weierstall, Uwe [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Doak, R. Bruce [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Schmidt, Kevin E. [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Wang, Xiaoyu [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Spence, John C. H. [Arizona State Univ., Tempe, AZ (United States). Dept. of Physics; Schlichting, Ilme [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Epp, Sascha W. [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Rolles, Daniel [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Rudenko, Artem [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Foucar, Lutz [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Rudek, Benedikt [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Erk, Benjamin [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Schmidt, Carlo [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Hömke, André [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Strüder, Lothar [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Society Semiconductor Lab., Munich (Germany); Ullrich, Joachim [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Krasniqi, Faton [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, Max Planck Advanced Study Group; Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Lomb, Lukas [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Shoeman, Robert L. [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Bott, Mario [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Barends, Thomas R. M. [Max Planck Inst. fur Medizinische Forschung, Heidelberg (Germany); Kuhnel, Kai-Uwe [Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Schroter, Claus-Dieter [Max Planck Inst. fur Kernphysik, Heidelberg (Germany); Hartmann, Robert [PNSensor GmbH, Munich (Germany); Holl, Peter [PNSensor GmbH, Munich (Germany); Reich, Christian [PNSensor GmbH, Munich (Germany); Soltau, Heike [PNSensor GmbH, Munich (Germany); Kimmel, Nils [Max Planck Society Semiconductor Lab., Munich (Germany); Weidenspointner, Georg [Max Planck Society Semiconductor Lab., Munich (Germany); Max Planck Inst. fur Extraterrestrische Physik, Garching (Germany); Pietschner, Daniel [Max Planck Society Semiconductor Lab., Munich (Germany); Hauser, Günter [Max Planck Society Semiconductor Lab., Munich (Germany); Herrmann, Sven [Max Planck Society Semiconductor Lab., Munich (Germany); Schaller, Gerhard [Max Planck Society Semiconductor Lab., Munich (Germany); Schopper, Florian [Max Planck Society Semiconductor Lab., Munich (Germany); Andritschke, Robert [Max Planck Society Semiconductor Lab., Munich (Germany); Boutet, Sébastien [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Krzywinski, Jacek [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Bostedt, Christoph [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Messerschmidt, Marc [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Bozek, John D. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Williams, Garth J. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Linac Coherent Light Source (LCLS); Bogan, Michael J. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Hampton, Christina Y. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Sierra, Raymond G. [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Starodub, Dmitri [SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE); Gorke, Hubert [Forschungszentrum Julich (Germany); Hau-Riege, Stefan P. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Frank, Matthias [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Maia, Filipe R. N. C. [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Hajdu, Janos [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Timneanu, Nicusor [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Seibert, M. Marvin [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Andreasson, Jakob [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Rocker, Andrea [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Jönsson, Olof [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Svenda, Martin [Uppsala Univ. (Sweden). Dept. of Cell and Molecular Biology, Lab. of Molecular Biophysics; Holton, James M. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Marchesini, Stefano [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS); Neutze, Richard [Univ. of Gothenburg (Sweden). Dept. of Chemistry, Biochemistry and Biophysics; Schorb, Sebastian [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Rupp, Daniela [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Adolph, Marcus [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Gorkhover, Tais [Technische Univ. Berlin (Germany). Inst. fur Optik und Atomare Physik (IOAP); Andersson, Inger [Swedish Univ. of Agricultural Sciences, Uppsala Biomedical Centre, Uppsala, (Sweden). Dept. of Molecular Biology; Barthelmess, Miriam [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Bajt, Saša [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Hirsemann, Helmut [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Potdevin, Guillaume [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Graafsma, Heinz [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science; Nilsson, Björn [Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science

    2011-02-03

    X-ray crystallography provides the vast majority of macromolecular structures, but the success of the method relies on growing crystals of sufficient size. In conventional measurements, the necessary increase in X-ray dose to record data from crystals that are too small leads to extensive damage before a diffraction signal can be recorded. It is particularly challenging to obtain large, well-diffracting crystals of membrane proteins, for which fewer than 300 unique structures have been determined despite their importance in all living cells. Here we present a method for structure determination where single-crystal X-ray diffraction ‘snapshots’ are collected from a fully hydrated stream of nanocrystals using femtosecond pulses from a hard-X-ray free-electron laser, the Linac Coherent Light Source. We prove this concept with nanocrystals of photosystem I, one of the largest membrane protein complexes. More than 3,000,000 diffraction patterns were collected in this study, and a three-dimensional data set was assembled from individual photosystem I nanocrystals (~200 nm to 2 μm in size). We mitigate the problem of radiation damage in crystallography by using pulses briefer than the timescale of most damage processes. This offers a new approach to structure determination of macromolecules that do not yield crystals of sufficient size for studies using conventional radiation sources or are particularly sensitive to radiation damage.

  19. Radio-protective effect of cinnamic acid, a phenolic phytochemical, on genomic instability induced by X-rays in human blood lymphocytes in vitro.

    Science.gov (United States)

    Cinkilic, Nilufer; Tüzün, Ece; Çetintaş, Sibel Kahraman; Vatan, Özgür; Yılmaz, Dilek; Çavaş, Tolga; Tunç, Sema; Özkan, Lütfi; Bilaloğlu, Rahmi

    2014-08-01

    The present study was designed to determine the protective activity of cinnamic acid against induction by X-rays of genomic instability in normal human blood lymphocytes. This radio-protective activity was assessed by use of the cytokinesis-block micronucleus test and the alkaline comet assay, with human blood lymphocytes isolated from two healthy donors. A Siemens Mevatron MD2 (Siemens AG, USA, 1994) linear accelerator was used for the irradiation with 1 or 2 Gy. Treatment of the lymphocytes with cinnamic acid prior to irradiation reduced the number of micronuclei when compared with that in control samples. Treatment with cinnamic acid without irradiation did not increase the number of micronuclei and did not show a cytostatic effect in the lymphocytes. The results of the alkaline comet assay revealed that cinnamic acid reduces the DNA damage induced by X-rays, showing a significant radio-protective effect. Cinnamic acid decreased the frequency of irradiation-induced micronuclei by 16-55% and reduced DNA breakage by 17-50%, as determined by the alkaline comet assay. Cinnamic acid may thus act as a radio-protective compound, and future studies may focus on elucidating the mechanism by which cinnamic acid offers radioprotection.

  20. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive medical ...

  1. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose ... limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is ...

  2. Lumbosacral spine x-ray

    Science.gov (United States)

    X-ray - lumbosacral spine; X-ray - lower spine ... The test is done in a hospital x-ray department or your health care provider's office by an x-ray technician. You will be asked to lie on the x-ray table ...

  3. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  4. Abdomen X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a very ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  5. X-ray lasers

    CERN Document Server

    Elton, Raymond C

    2012-01-01

    The first in its field, this book is both an introduction to x-ray lasers and a how-to guide for specialists. It provides new entrants and others interested in the field with a comprehensive overview and describes useful examples of analysis and experiments as background and guidance for researchers undertaking new laser designs. In one succinct volume, X-Ray Lasers collects the knowledge and experience gained in two decades of x-ray laser development and conveys the exciting challenges and possibilities still to come._Add on for longer version of blurb_M>The reader is first introduced

  6. X-Ray Diffraction.

    Science.gov (United States)

    Smith, D. K.; Smith, K. L.

    1980-01-01

    Reviews applications in research and analytical characterization of compounds and materials in the field of X-ray diffraction, emphasizing new developments in applications and instrumentation in both single crystal and powder diffraction. Cites 414 references. (CS)

  7. Medical X-Rays

    Science.gov (United States)

    ... The Conference of Radiation Control Program Directors (CRCPD) publishes Suggested State Regulations for the Control of Radiation , ... eSubmitter Guidance for Industry and Food and Drug Administration Staff - Assembler's Guide to Diagnostic X-Ray Equipment ...

  8. Chest X-Ray

    Medline Plus

    Full Text Available ... However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs any risk. ...

  9. Chest X-Ray

    Medline Plus

    Full Text Available ... chest x-ray is used to evaluate the lungs, heart and chest wall and may be used ... diagnose and monitor treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A ...

  10. X-ray diffraction study of Penicillium Vitale catalase in the complex with aminotriazole

    Science.gov (United States)

    Borovik, A. A.; Grebenko, A. I.; Melik-Adamyan, V. R.

    2011-07-01

    The three-dimensional structure of the enzyme catalase from Penicillium vitale in a complex with the inhibitor aminotriazole was solved and refined by protein X-ray crystallography methods. An analysis of the three-dimensional structure of the complex showed that the inhibition of the enzyme occurs as a result of the covalent binding of aminotriazole to the amino-acid residue His64 in the active site of the enzyme. An investigation of the three-dimensional structure of the complex resulted in the amino-acid residues being more precisely identified. The binding sites of saccharide residues and calcium ions in the protein molecule were found.

  11. X-ray diffraction study of Penicillium Vitale catalase in the complex with aminotriazole

    International Nuclear Information System (INIS)

    The three-dimensional structure of the enzyme catalase from Penicillium vitale in a complex with the inhibitor aminotriazole was solved and refined by protein X-ray crystallography methods. An analysis of the three-dimensional structure of the complex showed that the inhibition of the enzyme occurs as a result of the covalent binding of aminotriazole to the amino-acid residue His64 in the active site of the enzyme. An investigation of the three-dimensional structure of the complex resulted in the amino-acid residues being more precisely identified. The binding sites of saccharide residues and calcium ions in the protein molecule were found.

  12. X-ray diffraction study of Penicillium Vitale catalase in the complex with aminotriazole

    Energy Technology Data Exchange (ETDEWEB)

    Borovik, A. A.; Grebenko, A. I.; Melik-Adamyan, V. R., E-mail: mawr@ns.crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2011-07-15

    The three-dimensional structure of the enzyme catalase from Penicillium vitale in a complex with the inhibitor aminotriazole was solved and refined by protein X-ray crystallography methods. An analysis of the three-dimensional structure of the complex showed that the inhibition of the enzyme occurs as a result of the covalent binding of aminotriazole to the amino-acid residue His64 in the active site of the enzyme. An investigation of the three-dimensional structure of the complex resulted in the amino-acid residues being more precisely identified. The binding sites of saccharide residues and calcium ions in the protein molecule were found.

  13. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  14. X-ray structure of 1D-coordination polymer of copperII bearing 1,4-pyrazine-2,3-dicarboxylic acid and 2-aminopyrimidine

    OpenAIRE

    Mirzaei Masoud; Eshtiagh-Hosseini Hossein; Hassanpoor Azam; Barba Victor

    2012-01-01

    The new 1D-coordination polymer of CuII ion, {(2- apymH)2[Cu(pyzdc)2] .6H2O}n, (2-apym = 2-aminopyrimidine, pyzdcH2 = 1,4- pyrazine-2,3-dicarboxylic acid), was synthesized based on proton transfer mechanism and characterized by elemental analysis, infrared spectroscopy, and single crystal X-ray diffraction. The coordination polymer consists of infinite anionic chains of [Cu(pyzdc)2]2- anion bridged crossing double chain running along a-axis and discrete (2-apymH)+ fragment. The CuII ion...

  15. X-ray Pulsars

    CERN Document Server

    Walter, Roland

    2016-01-01

    X-ray pulsars shine thanks to the conversion of the gravitational energy of accreted material to X-ray radiation. The accretion rate is modulated by geometrical and hydrodynamical effects in the stellar wind of the pulsar companions and/or by instabilities in accretion discs. Wind driven flows are highly unstable close to neutron stars and responsible for X-ray variability by factors $10^3$ on time scale of hours. Disk driven flows feature slower state transitions and quasi periodic oscillations related to orbital motion and precession or resonance. On shorter time scales, and closer to the surface of the neutron star, X-ray variability is dominated by the interactions of the accreting flow with the spinning magnetosphere. When the pulsar magnetic field is large, the flow is confined in a relatively narrow accretion column, whose geometrical properties drive the observed X-ray emission. In low magnetized systems, an increasing accretion rate allows the ignition of powerful explosive thermonuclear burning at t...

  16. Incoherent x-ray scattering in single molecule imaging

    CERN Document Server

    Slowik, Jan Malte; Dixit, Gopal; Jurek, Zoltan; Santra, Robin

    2014-01-01

    Imaging of the structure of single proteins or other biomolecules with atomic resolution would be enormously beneficial to structural biology. X-ray free-electron lasers generate highly intense and ultrashort x-ray pulses, providing a route towards imaging of single molecules with atomic resolution. The information on molecular structure is encoded in the coherent x-ray scattering signal. In contrast to crystallography there are no Bragg reflections in single molecule imaging, which means the coherent scattering is not enhanced. Consequently, a background signal from incoherent scattering deteriorates the quality of the coherent scattering signal. This background signal cannot be easily eliminated because the spectrum of incoherently scattered photons cannot be resolved by usual scattering detectors. We present an ab initio study of incoherent x-ray scattering from individual carbon atoms, including the electronic radiation damage caused by a highly intense x-ray pulse. We find that the coherent scattering pa...

  17. X-ray astronomy

    International Nuclear Information System (INIS)

    This book contains the lectures, and the most important seminars held at the NATO meeting on X-Ray astronomy in Erice, July 1979. The meeting was an opportune forum to discuss the results of the first 8-months of operation of the X-ray satellite, HEAO-2 (Einstein Observatory) which was launched at the end of 1978. Besides surveying these results, the meeting covered extragalactic astronomy, including the relevant observations obtained in other portions of the electromagnetic spectrum (ultra-violet, optical, infrared and radio). The discussion on galactic X-ray sources essentially covered classical binaries, globular clusters and bursters and its significance to extragalactic sources and to high energy astrophysics was borne in mind. (orig.)

  18. CRL X-RAY TUBE

    OpenAIRE

    Kolchevsky, N. N.; Petrov, P. V.

    2015-01-01

    A novel types of X-ray tubes with refractive lenses are proposed. CRL-R X-ray tube consists of Compound Refractive Lens- CRL and Reflection X-ray tube. CRL acts as X-ray window. CRL-T X-ray consists of CRL and Transmission X-ray tube. CRL acts as target for electron beam. CRL refractive lens acts as filter, collimator, waveguide and focusing lens. Properties and construction of the CRL X-ray tube are discussed.

  19. Aqueous solubility study of salts of benzylamine derivatives and p-substituted benzoic acid derivatives using X-ray crystallographic analysis

    DEFF Research Database (Denmark)

    Parshad, Henrik; Frydenvang, Karla Andrea; Liljefors, Tommy;

    2004-01-01

    Twenty two p-substituted benzoic acid derivates were used to prepare salts of N-methylbenzylamine (II) and N,N-dimethylbenzylamine (III), respectively. Only five salts of (II) and two salts of (III) were obtained in a crystalline state. The solubility of these salts was orders of magnitude higher...... than those reported for the corresponding salts of benzylamine (I). Thermal analysis indicated that the increased solubility was caused by reduced crystal lattice energy, which was most likely due to the reduced number of strong hydrogen bonds of the salt of (II) and (III). X-ray crystallographic...... analysis of p-hydroxybenzoic acid salt of (I), (II) and (III) suggested that the reduced number of hydrogen bonds caused the apparent higher solubility. Further analyses of seven salts of (I) were performed. It was not possible to identify any relationship between the number of hydrogen bonds...

  20. Low-temperature phase transition in glycine-glutaric acid co-crystals studied by single-crystal X-ray diffraction, Raman spectroscopy and differential scanning calorimetry.

    Science.gov (United States)

    Zakharov, Boris A; Losev, Evgeniy A; Kolesov, Boris A; Drebushchak, Valeri A; Boldyreva, Elena V

    2012-06-01

    The occurrence of a first-order reversible phase transition in glycine-glutaric acid co-crystals at 220-230 K has been confirmed by three different techniques - single-crystal X-ray diffraction, polarized Raman spectroscopy and differential scanning calorimetry. The most interesting feature of this phase transition is that every second glutaric acid molecule changes its conformation, and this fact results in the space-group symmetry change from P2(1)/c to P1. The topology of the hydrogen-bonded motifs remains almost the same and hydrogen bonds do not switch to other atoms, although the hydrogen bond lengths do change and some of the bonds become inequivalent.

  1. X-ray structure of 1D-coordination polymer of copperII bearing 1,4-pyrazine-2,3-dicarboxylic acid and 2-aminopyrimidine

    Directory of Open Access Journals (Sweden)

    Mirzaei Masoud

    2012-01-01

    Full Text Available The new 1D-coordination polymer of CuII ion, {(2- apymH2[Cu(pyzdc2] .6H2O}n, (2-apym = 2-aminopyrimidine, pyzdcH2 = 1,4- pyrazine-2,3-dicarboxylic acid, was synthesized based on proton transfer mechanism and characterized by elemental analysis, infrared spectroscopy, and single crystal X-ray diffraction. The coordination polymer consists of infinite anionic chains of [Cu(pyzdc2]2- anion bridged crossing double chain running along a-axis and discrete (2-apymH+ fragment. The CuII ion is located on inversion centre in the basal plane of an elongated octahedron and two oxygen atoms from adjacent (pyzdc2-ligands occupy axial position. The interaction between oxygen atoms of water molecules along with the dicarboxylic acid play an important role in the overall supramolecular assembly.

  2. Chest X-Ray

    Medline Plus

    Full Text Available ... this Site RadiologyInfo.org is produced by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript ... time! Spotlight Recently posted: Pediatric MRI Intravascular Ultrasound Video: Chest CT Video:Thyroid Ultrasound Video: Head CT ...

  3. Chest X-Ray

    Medline Plus

    Full Text Available ... Pediatric Ultrasound Video: Angioplasty & vascular stenting Video: Arthrography Radiology and You About this Site RadiologyInfo.org is ... radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey ...

  4. Chest X-Ray

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    Full Text Available ... this Site RadiologyInfo.org is produced by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript ... Recently posted: Focused Ultrasound for Uterine Fibroids Dementia Video: General Ultrasound Video: Pediatric Nuclear Medicine Radiology and ...

  5. Medical x-ray

    International Nuclear Information System (INIS)

    This book describes the fundamental subject about medical radiography. It is a multidisciplinary field that requires cross professional input from scientists, engineers and medical doctors. However, it is presented in simple language to suit different levels of readers from x-ray operators and radiographers to physists, general practitioners and radiology specialists.The book is written in accordance to the requirements of the standard syllabus approved by the Ministry of Health Malaysia for the training of medical x-ray operator and general practitioners. In general, the content is not only designed to provide relevant and essential subject for related professionals in medical radiological services such as x-ray operator, radiographer and radiologists, but also to address those in associated radiological services including nurses, medical technologists and physicists.The book is organized and arranged sequentially into 3 parts for easy reference: Radiation safety; X-ray equipment and associated facilities; Radiography practices. With proper grasping of all these parts, the radiological services could be provided with confident and the highest professional standard. Thus, medical imaging with highest quality that can provide useful diagnostic information at minimum doses and at cost effective could be assured

  6. Powder X-ray diffraction study af alkali alanates

    DEFF Research Database (Denmark)

    Cao, Thao; Mosegaard Arnbjerg, Lene; Jensen, Torben René

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...

  7. Pyroelectric x-ray detectors and x-ray pyrometers

    International Nuclear Information System (INIS)

    This paper discusses pyroelectric detectors which are very promising x-ray detectors for intense pulsed x-ray/γ-ray measurements and can be used as x-ray pyrometers. They are fast, passive, and inherently flat in spectral response for low energy x-rays. The authors report tests of LiTaO3, Sr.5Ba.5Nb2O6 and LiNbO3 detectors at Nova laser with 1 ns low energy x-rays and at Zapp Z-pinch machine with 100 ns x-rays. The temporal and spectral responses are discussed

  8. Pyroelectric x-ray detectors and x-ray pyrometers

    International Nuclear Information System (INIS)

    Pyroelectric detectors are very promising x-ray detectors for intense pulsed x-ray/γ-ray measurements and can be used as x-ray pyrometers. They are fast, passive, and inherently flat in spectral response for low-energy x rays. We report our tests of LiTaO3 detectors at Nova laser with 1-ns low-energy x rays and at Zapp Z-pinch machine with 100-ns x rays. The temporal and spectral responses are discussed

  9. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    Science.gov (United States)

    Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

    2015-07-01

    Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

  10. Fourier-Transform Ghost Imaging with Hard X Rays

    Science.gov (United States)

    Yu, Hong; Lu, Ronghua; Han, Shensheng; Xie, Honglan; Du, Guohao; Xiao, Tiqiao; Zhu, Daming

    2016-09-01

    Knowledge gained through x-ray crystallography fostered structural determination of materials and greatly facilitated the development of modern science and technology in the past century. However, it is only applied to crystalline structures and cannot resolve noncrystalline materials. Here we demonstrate a novel lensless Fourier-transform ghost imaging method with pseudothermal hard x rays that extends x-ray crystallography to noncrystalline samples. By measuring the second-order intensity correlation function of the light, Fourier-transform diffraction pattern of a complex amplitude sample is achieved at the Fresnel region in our experiment and the amplitude and phase distributions of the sample in the spatial domain are retrieved successfully. For the first time, ghost imaging is experimentally realized with x rays. Since a highly coherent x-ray source is not required, the method can be implemented with laboratory x-ray sources and it also provides a potential solution for lensless diffraction imaging with fermions, such as neutrons and electrons where intensive coherent sources usually are not available.

  11. Fourier-transform Ghost Imaging with Hard X-rays

    CERN Document Server

    Yu, Hong; Han, Shensheng; Xie, Honglan; Du, Guohao; Xiao, Tiqiao; Zhu, Daming

    2016-01-01

    Knowledge gained through X-ray crystallography fostered structural determination of materials and greatly facilitated the development of modern science and technology in the past century. Atomic details of sample structures is achievable by X-ray crystallography, however, it is only applied to crystalline structures. Imaging techniques based on X-ray coherent diffraction or zone plates are capable of resolving the internal structure of non-crystalline materials at nanoscales, but it is still a challenge to achieve atomic resolution. Here we demonstrate a novel lensless Fourier-transform ghost imaging method with pseudo-thermal hard X-rays by measuring the second-order intensity correlation function of the light. We show that high resolution Fourier-transform diffraction pattern of a complex structure can be achieved at Fresnel region, and the amplitude and phase distributions of a sample in spatial domain can be retrieved successfully. The method of lensless X-ray Fourier-transform ghost imaging extends X-ray...

  12. The structure investigations of dehydroacetic acid and 1,8-diaminonaphthalene condensation product by NMR, MS, and X-ray measurements

    Science.gov (United States)

    Kołodziej, B.; Morawiak, M.; Kamieński, B.; Schilf, W.

    2016-05-01

    A new unexpected product of condensation reaction of 1,8-diaminonaphthalene (DAN) and carbonyl compound (here: dehydroacetic acid (dha)) was synthesized. Discussion about the molecular structure of possible products of this reaction was done on the base of NMR studies. The structure of the titled product in both DMSO solution and in the solid state was resolved by analysis of its spectral data (X-ray structure analysis, multinuclear NMR in solution and solid state spectra) and MS measurements. The presented studies provided clear evidence that the titled product exists in diluted DMSO solution as the mixture of two kinetic free ionic species whereas in concentrated DMSO solution as well as in the solid state this system forms associated ionic pairs bonded together by hydrogen bonds.

  13. Leaf-cutting ants toxicity of limonexic acid and degraded limonoids from Raulinoa echinata: X-ray structure of epoxy-fraxinellone

    Energy Technology Data Exchange (ETDEWEB)

    Biavatti, Maique W.; Westerlon, Rosangela [Universidade do Vale do Itajai, SC (Brazil). Programa de Pos-Graduacao em Ciencias Farmaceuticas]. E-mail: maique@univali.br; Vieira, Paulo C.; Silva, M. Fatima G.F. da; Fernandes, Joao B. [Sao Carlos Univ., SP (Brazil). Dept. de Quimica; Penaflor, M. Fernanda G.V.; Bueno, Odair C. [UNESP, Rio Claro, SP (Brazil). Centro de Estudos de Insetos Sociais; Ellena, Javier [Sao Paulo Univ., Sao Carlos, SP (Brazil). Inst. de Fisica

    2005-11-15

    Phytochemical survey of roots extracts of the South Brazilian endemic plant Raulinoa echinata Cowan, Rutaceae led to the isolation of known degraded limonoids: fraxinellone, fraxinellonone and epoxy-fraxinellone. The latter was previously isolated also from the stems, but the relative configuration could not be solved by NMR experiments. This paper deals with the X-ray diffraction analysis of epoxy-fraxinellone and its toxicity to leaf-cutting ants, describes the isolation of fraxinellonone and fraxinellone for the first time in Raulinoa. Epoxy-fraxinellone showed no toxicity to the leaf-cutting ants (Atta sexdens rubropilosa). The limonoid limonexic acid, isolated from stems, presented high toxicity to the leaf-cutting ants, diminishing considerably their longevity. (author)

  14. Coherent convergent-beam time-resolved X-ray diffraction

    OpenAIRE

    Spence, John C. H.; Zatsepin, Nadia A.; Li, Chufeng

    2014-01-01

    The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic ...

  15. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... wrist, arm, elbow, shoulder, spine, pelvis, hip, thigh, knee, leg (shin), ankle or foot. top of page ... the patient standing upright, as in cases of knee x-rays. A portable x-ray machine is ...

  16. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... images for evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ...

  17. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... fracture. guide orthopedic surgery, such as spine repair/fusion, joint replacement and fracture reductions. look for injury, ... and Media Arthritis X-ray, Interventional Radiology and Nuclear Medicine Radiation Safety Images related to X-ray ( ...

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and ...

  19. Dental X-ray apparatus

    International Nuclear Information System (INIS)

    Intra-oral dental X-ray apparatus for panoramic radiography is described in detail. It comprises a tubular target carrier supporting at its distal end a target with an inclined forward face. Image definition is improved by positioning in the path of the X-rays a window of X-ray transmitting ceramic material, e.g. 90% oxide of Be, or Al, 7% Si02. The target carrier forms a probe which can be positioned in the patient's mouth. X-rays are directed forwardly and laterally of the target to an X-ray film positioned externally. The probe is provided with a detachable sleeve having V-form arms of X-ray opaque material which serve to depress the tongue out of the radiation path and also shield the roof of the mouth and other regions of the head from the X-ray pattern. A cylindrical lead shield defines the X-ray beam angle. (author)

  20. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ...

  1. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... As a result, bones appear white on the x-ray, soft tissue shows up in shades of gray and air appears black. Until recently, x-ray images were maintained on large film sheets (much ...

  2. Panoramic Dental X-Ray

    Science.gov (United States)

    ... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a ... a large photographic negative). Today, most images are digital files that are stored electronically. These stored images ...

  3. Characterization of D-glucaric acid using NMR, x-ray crystal structure, and MM3 molecular modeling analyses

    Science.gov (United States)

    D-glucaric acid was characterized in solution by comparing NMR spectra from the isotopically unlabeled molecule with those from D-glucaric acid labeled with deuterium or carbon-13 atoms. The NMR studies provided unequivocal assignments for all carbon atoms and non-hydroxyl protons of the molecule. ...

  4. Phosphole complexes of Gold(I) halides: Comparison of solution and solid-state structures by a combination of solution and CP/MAS 31P NMR spectroscopy and x-ray crystallography

    International Nuclear Information System (INIS)

    A series of complexes of 1-phenyldibenzophosphole (DBP), 1-phenyl-3,4,-dimethylphosphole (DMPP), and triphenylphosphine of the type LnAuX (n = 1, L = DBP, DMPP, Ph3P, X = Cl, Br, I; n = 3, L = DBP, X = Cl, Br, I; n = 3, L = Ph3P, X = Cl; n = 4, L = DBP, DMPP, X = PF6) have been prepared and characterized. The structures of (DBP)AuCl (1), (DBP)3AuCl (2), and (DMPP)AuCl (3) have been determined from three-dimensional x-ray data collected by counter methods. Crystal structure of the complexes is reported. The CP/MAS 31P(1H) NMR spectrum of complex 1 shows two resonances in a 1:1 intensity ratio, and the CP/MAS 31P(1H) NMR spectrum of complex 3 shows three resonances in a 1:1:1 intensity ratio for reasons that are not yet understood. Though the three phospholes are crystallographically inequivalent (d(AuP) = 2.359 (1), 2.382 (1), and 2.374 (2) angstrom) the molecule has effective Cs symmetry as evidenced by the observation of two 31P resonances in a 2:1 intensity ratio in its CP/MAS 31P(1H) NMR spectrum. Variable-temperature 31P(1H) NMR spectra obtained on solutions of LAuCl + L in various ratios were analyzed to determine the nature of the species present in solution and to gain information regarding their relative stabilities as a function of the nature of the phosphine. 79 refs., 8 figs., 9 tabs

  5. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... x-rays. top of page What does the equipment look like? The equipment typically used for bone x-rays consists of ... and joint abnormalities, such as arthritis. X-ray equipment is relatively inexpensive and widely available in emergency ...

  6. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... The x-ray tube is connected to a flexible arm that is extended over the patient while an x-ray film holder or image recording plate is placed beneath the patient. top of page How does the procedure work? X-rays are a form of radiation like ...

  7. Tunable X-ray source

    Science.gov (United States)

    Boyce, James R.

    2011-02-08

    A method for the production of X-ray bunches tunable in both time and energy level by generating multiple photon, X-ray, beams through the use of Thomson scattering. The method of the present invention simultaneously produces two X-ray pulses that are tunable in energy and/or time.

  8. X-ray selected BALQSOs

    CERN Document Server

    Page, M J; Ceballos, M; Corral, A; Ebrero, J; Esquej, P; Krumpe, M; Mateos, S; Rosen, S; Schwope, A; Streblyanska, A; Symeonidis, M; Tedds, J A; Watson, M G

    2016-01-01

    We study a sample of six X-ray selected broad absorption line (BAL) quasi-stellar objects (QSOs) from the XMM-Newton Wide Angle Survey. All six objects are classified as BALQSOs using the classic balnicity index, and together they form the largest sample of X-ray selected BALQSOs. We find evidence for absorption in the X-ray spectra of all six objects. An ionized absorption model applied to an X-ray spectral shape that would be typical for non-BAL QSOs (a power law with energy index alpha=0.98) provides acceptable fits to the X-ray spectra of all six objects. The optical to X-ray spectral indices, alpha_OX, of the X-ray selected BALQSOs, have a mean value of 1.69 +- 0.05, which is similar to that found for X-ray selected and optically selected non-BAL QSOs of similar ultraviolet luminosity. In contrast, optically-selected BALQSOs typically have much larger alpha_OX and so are characterised as being X-ray weak. The results imply that X-ray selection yields intrinsically X-ray bright BALQSOs, but their X-ray sp...

  9. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... lies. A drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... that is extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  10. X-Ray Exam: Ankle

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Ankle KidsHealth > For Parents > X-Ray Exam: Ankle Print A A A Text Size ... español Radiografía: tobillo What It Is An ankle X-ray is a safe and painless test that uses ...

  11. X-Ray Exam: Finger

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Finger KidsHealth > For Parents > X-Ray Exam: Finger Print A A A Text Size ... español Radiografía: dedo What It Is A finger X-ray is a safe and painless test that uses ...

  12. X-Ray Exam: Wrist

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Wrist KidsHealth > For Parents > X-Ray Exam: Wrist Print A A A Text Size ... español Radiografía: muñeca What It Is A wrist X-ray is a safe and painless test that uses ...

  13. X-Ray Exam: Hip

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Hip KidsHealth > For Parents > X-Ray Exam: Hip Print A A A Text Size ... español Radiografía: cadera What It Is A hip X-ray is a safe and painless test that uses ...

  14. X-Ray Exam: Forearm

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Forearm KidsHealth > For Parents > X-Ray Exam: Forearm Print A A A Text Size ... español Radiografía: brazo What It Is A forearm X-ray is a safe and painless test that uses ...

  15. X-Ray Exam: Pelvis

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Pelvis KidsHealth > For Parents > X-Ray Exam: Pelvis Print A A A Text Size ... español Radiografía: pelvis What It Is A pelvis X-ray is a safe and painless test that uses ...

  16. X-Ray Exam: Foot

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Foot KidsHealth > For Parents > X-Ray Exam: Foot Print A A A Text Size ... español Radiografía: pie What It Is A foot X-ray is a safe and painless test that uses ...

  17. X-ray crystallographic, FT-IR and NMR studies as well as anticancer and antibacterial activity of the salt formed between ionophore antibiotic Lasalocid acid and amines

    Science.gov (United States)

    Huczyński, Adam; Rutkowski, Jacek; Wietrzyk, Joanna; Stefańska, Joanna; Maj, Ewa; Ratajczak-Sitarz, Małgorzata; Katrusiak, Andrzej; Brzezinski, Bogumil; Bartl, Franz

    2013-01-01

    Two new complexes of the ionophore antibiotic Lasalocid acid (LAS) with phenylamine (PhA) and butylamine (BuA) were synthesized and their molecular structures were studied using single crystal X-ray diffraction and spectroscopic methods. In the solid state both amines are protonated and all NH3+ protons are hydrogen bonded to etheric, hydroxyl and carboxylic oxygen atoms of the LAS anion. In chloroform solutions the structure observed in the crystal of LAS-BuA complex is preserved and an equilibrium between the LAS-PhA complex and dissociated Lasalocid acid and phenylamine is observed. In vitro antimicrobial tests of the complexes showed a significant activity towards some strains of Gram-positive bacteria. For the first time Lasalocid acid and its complexes with amines were tested in vitro for cytotoxic activity against human cancer cell lines: A-549 (lung), MCF-7 (breast), HT-29 (colon) and mouse cancer cell line P-388 (leukemia). We found that LAS and its complexes are strong cytotoxic agents towards all tested cell lines. The cytostatic activity of the compounds studied is greater than that of cisplatin, indicating that Lasalocid and its complexes are promising candidates for new anticancer drugs.

  18. X-ray today

    Energy Technology Data Exchange (ETDEWEB)

    Neitzel, U. [Philips Medical Systems, Hamburg (Germany)

    2001-09-01

    The interest attracted by the new imaging modalities tends to overshadow the continuing importance of projection radiography and fluoroscopy. Nevertheless, projection techniques still represent by far the greatest proportion of diagnostic imaging examinations, and play an essential role in the growing number of advanced interventional procedures. This article describes some of the latest developments in X-ray imaging technology, using two products from the Philips range as examples: the Integris Allura cardiovascular system with 3D image reconstruction, and the BV Pulsera: a high-end, multi-functional mobile C-arm system with cardiac capabilities. (orig.)

  19. The Microwave-assisted Preparation and X-Ray Structure of 3-Bromocarbazole-N-Acetic Acid

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The rapid synthesis of 3-bromocarbazole-N-acetic acid was performed using microwave irradiation. Under the optimal conditions the yield was 85.6 %. The crystal structure showed that the carboxylic groups form bifurcated hydrogen bonds and the hydroxyl oxygen atoms serve as proton donors and also acceptor. Each carboxylic group was involved in four hydrogen bonds. The packing of crystal was dominated by links of these hydrogen bonds.

  20. Expression, purification, crystallization and preliminary X-ray analysis of a novel N-substituted branched-chain l-amino-acid dioxygenase from Burkholderia ambifaria AMMD

    International Nuclear Information System (INIS)

    Diffraction data were collected to a limiting resolution of 2.4 Å from a crystal of selenomethionyl-labelled SadA, an l-amino-acid dioxygenase. Ferrous ion- and α-ketoglutarate-dependent dioxygenase from Burkholderia ambifaria AMMD (SadA) catalyzes the C3-hydroxylation of N-substituted branched-chain l-amino acids, especially N-succinyl-l-leucine, coupled to the conversion of α-ketoglutarate to succinate and CO2. SadA was expressed in Escherichia coli, purified and crystallized using the sitting-drop vapour-diffusion method at 293 K. Crystals of selenomethionine-substituted SadA were obtained using a reservoir solution containing PEG 3000 as the precipitant at pH 9.5 and diffracted X-rays to 2.4 Å resolution. The crystal belonged to space group P212121, with unit-cell parameters a = 49.3, b = 70.9, c = 148.2 Å. The calculated Matthews coefficient (VM = 2.1 Å3 Da−1, 41% solvent content) suggested that the crystal contains two molecules per asymmetric unit

  1. Characterization of the Adsorption of Nucleic Acid Bases onto Ferrihydrite via Fourier Transform Infrared and Surface-Enhanced Raman Spectroscopy and X-ray Diffractometry.

    Science.gov (United States)

    Canhisares-Filho, José E; Carneiro, Cristine E A; de Santana, Henrique; Urbano, Alexandre; da Costa, Antonio C S; Zaia, Cássia T B V; Zaia, Dimas A M

    2015-09-01

    Minerals could have played an important role in concentration, protection, and polymerization of biomolecules. Although iron is the fourth most abundant element in Earth's crust, there are few works in the literature that describe the use of iron oxide-hydroxide in prebiotic chemistry experiments. In the present work, the interaction of adenine, thymine, and uracil with ferrihydrite was studied under conditions that resemble those of prebiotic Earth. At acidic pH, anions in artificial seawater decreased the pH at the point of zero charge (pHpzc) of ferrihydrite; and at basic pH, cations increased the pHpzc. The adsorption of nucleic acid bases onto ferrihydrite followed the order adenine > uracil > thymine. Adenine adsorption peaked at neutral pH; however, for thymine and uracil, adsorption increased with increasing pH. Electrostatic interactions did not appear to play an important role on the adsorption of nucleic acid bases onto ferrihydrite. Adenine adsorption onto ferrihydrite was higher in distilled water compared to artificial seawater. After ferrihydrite was mixed with artificial seawaters or nucleic acid bases, X-ray diffractograms and Fourier transform infrared spectra did not show any change. Surface-enhanced Raman spectroscopy showed that the interaction of adenine with ferrihydrite was not pH-dependent. In contrast, the interactions of thymine and uracil with ferrihydrite were pH-dependent such that, at basic pH, thymine and uracil lay flat on the surface of ferrihydrite, and at acidic pH, thymine and uracil were perpendicular to the surface. Ferrihydrite adsorbed much more adenine than thymine; thus adenine would have been better protected against degradation by hydrolysis or UV radiation on prebiotic Earth. PMID:26393397

  2. Insights into Equilibrium Dynamics of Proteins from Comparison of NMR and X-Ray Data with Computational Predictions

    OpenAIRE

    Yang, Lee-Wei; Eyal, Eran; Chennubhotla, Chakra; Jee, JunGoo; Gronenborn, Angela M.; Bahar, Ivet

    2007-01-01

    For a representative set of 64 nonhomologous proteins, each containing a structure solved by NMR and X-ray crystallography, we analyzed the variations in atomic coordinates between NMR models, the temperature (B) factors measured by X-ray crystallography, and the fluctuation dynamics predicted by the Gaussian network model (GNM). The NMR and X-ray data exhibited a correlation of 0.49. The GNM results, on the other hand, yielded a correlation of 0.59 with X-ray data and a distinctively better ...

  3. Novel 2-oxoimidazolidine-4-carboxylic acid derivatives as Hepatitis C virus NS3-4A serine protease inhibitors: synthesis, activity, and X-ray crystal structure of an enzyme inhibitor complex

    Energy Technology Data Exchange (ETDEWEB)

    Arasappan, Ashok; Njoroge, F. George; Parekh, Tejal N.; Yang, Xiaozheng; Pichardo, John; Butkiewicz, Nancy; Prongay, Andrew; Yao, Nanhua; Girijavallabhan, Viyyoor (SPRI)

    2008-06-30

    Synthesis and HCV NS3 serine protease inhibitory activity of some novel 2-oxoimidazolidine-4-carboxylic acid derivatives are reported. Inhibitors derived from this new P2 core exhibited activity in the low {micro}M range. X-ray structure of an inhibitor, 15c bound to the protease is presented.

  4. Quantum effets in nonresonant X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Slowik, Jan Malte

    2015-11-15

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  5. Quantum effets in nonresonant X-ray scattering

    International Nuclear Information System (INIS)

    Due to their versatile properties, X rays are a unique tool to investigate the structure and dynamics of matter. X-ray scattering is the fundamental principle of many imaging techniques. Examples are X-ray crystallography, which recently celebrated one hundred years and is currently the leading method in structure determination of proteins, as well as X-ray phase contrast imaging (PCI), which is an imaging technique with countless applications in biology, medicine, etc. The technological development of X-ray free electron lasers (XFEL) has brought X-ray imaging at the edge of a new scientific revolution. XFELs offer ultrashort X-ray pulses with unprecedented high X-ray fluence and excellent spatial coherence properties. These properties make them an outstanding radiation source for X-ray scattering experiments, providing ultrafast temporal resolution as well as atomic spatial resolution. However, the radiation-matter interaction in XFEL experiments also advances into a novel regime. This demands a sound theoretical fundament to describe and explore the new experimental possibilities. This dissertation is dedicated to the theoretical study of nonresonant X-ray scattering. As the first topic, I consider the near-field imaging by propagation based X-ray phase contrast imaging (PCI). I devise a novel theory of PCI, in which radiation and matter are quantized. Remarkably, the crucial interference term automatically excludes contributions from inelastic scattering. This explains the success of the classical description thus far. The second topic of the thesis is the X-ray imaging of coherent electronic motion, where quantum effects become particularly apparent. The electron density of coherent electronic wave packets - important in charge transfer and bond breaking - varies in time, typically on femto- or attosecond time scales. In the near future, XFELs are envisaged to provide attosecond X-ray pulses, opening the possibility for time-resolved ultrafast X-ray scattering

  6. In situ SERS and X-ray photoelectron spectroscopy studies on the pH-dependant adsorption of anthraquinone-2-carboxylic acid on silver electrode

    Science.gov (United States)

    Li, Dan; Jia, Shaojie; Fodjo, Essy Kouadio; Xu, Hu; Wang, Yuhong; Deng, Wei

    2016-03-01

    In this study, in situ surface-enhanced Raman scattering (SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS) are used to investigate the redox reaction and adsorption behavior of anthraquinone-2-carboxylic acid (AQ-2-COOH) on an Ag electrode at different pH values. The obtained results indicate that AQ-2-COOH is adsorbed tilted on the Ag electrode through O-atom of ring carbonyl in a potential range from -0.3 to -0.5 V vs. SCE, but the orientation turns to more tilted orientation with both O-atom of the ring carbonyl and carboxylate group in positive potential region for pH 6.0 and 7.4. However, at pH 10.0, the orientation adopts tilted conformation constantly on the Ag electrode with both O-atom of the anthraquinone ring and carboxylate group in the potential range from -0.3 to -0.5 V vs. SCE or at positive potentials. Moreover, the adsorption behavior of AQ-2-COOH has been further confirmed by AR-XPS on the Ag surface. Proposed reasons for the observed changes in orientation are presented.

  7. Expression, purification, crystallization and preliminary X-ray diffraction analysis of the VP8* sialic acid-binding domain of porcine rotavirus strain OSU

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yang-De, E-mail: zhangyd1960@yahoo.com.cn; Li, Hao [National Hepatobiliary and Enteric Surgery Research Center of The Ministry of Health, Xiangya Hospital, Central South University, Hunan Province (China); Liu, Hui; Pan, Yi-Feng [Biochemistry Laboratory, Institution of Biomedical Engineering, Central South University, Hunan Province (China); National Hepatobiliary and Enteric Surgery Research Center of The Ministry of Health, Xiangya Hospital, Central South University, Hunan Province (China)

    2007-02-01

    Porcine rotavirus strain OSU VP8* domain has been expressed, purified and crystallized. X-ray diffraction data from different crystal forms of the VP8* domain have been collected to 2.65 and 2.2 Å resolution, respectively. The rotavirus outer capsid spike protein VP4 is utilized in the process of rotavirus attachment to and membrane penetration of host cells. VP4 is cleaved by trypsin into two domains: VP8* and VP5*. The VP8* domain is implicated in initial interaction with sialic acid-containing cell-surface carbohydrates and triggers subsequent virus invasion. The VP8* domain from porcine OSU rotavirus was cloned and expressed in Escherichia coli. Different crystal forms (orthorhombic P2{sub 1}2{sub 1}2{sub 1} and tetragonal P4{sub 1}2{sub 1}2) were harvested from two distinct crystallization conditions. Diffraction data have been collected to 2.65 and 2.2 Å resolution and the VP8*{sub 65–224} structure was determined by molecular replacement.

  8. Topological X-Rays Revisited

    Science.gov (United States)

    Lynch, Mark

    2012-01-01

    We continue our study of topological X-rays begun in Lynch ["Topological X-rays and MRI's," iJMEST 33(3) (2002), pp. 389-392]. We modify our definition of a topological magnetic resonance imaging and give an affirmative answer to the question posed there: Can we identify a closed set in a box by defining X-rays to probe the interior and without…

  9. Crystallization and preliminary X-ray investigation of proteinase A, a non-pepsin-type acid proteinase from Aspergillus niger var. macrosporus.

    Science.gov (United States)

    Tanokura, M; Matsuzaki, H; Iwata, S; Nakagawa, A; Hamaya, T; Takizawa, T; Takahashi, K

    1992-01-01

    Proteinase A from Aspergillus niger var. macrosporus is a non-pepsin-type acid proteinase distinctly different in various properties from the family of pepsin-type aspartic proteinases, and so far it remains unknown which residues participate in the catalysis of the enzyme and how the mechanism operates. The acid proteinase A was crystallized from an ammonium sulfate solution by the hanging-drop vapor diffusion method. The space group of the crystals was P2(1)2(1)2(1) with unit cell dimensions of a = 54.7 A, b = 70.4 A and c = 38.0 A. On the assumption that there is one enzyme molecule in the asymmetric unit, the calculated ratio of volume to unit protein mass (Vm) was 1.64 A3 per dalton. Diffraction data were collected up to a resolution higher than 1.5 A, using the Weissenberg camera for macromolecular crystallography with synchrotron radiation. The crystal of proteinase A is, therefore, suitable for the structural analysis with a high resolution.

  10. X-ray lithography sources

    International Nuclear Information System (INIS)

    Synchrotron from dipole magnets in electron storage rings has emerged as a useful source of x-rays for lithography. To meet the need for these sources numerous groups around the world have embarked on projects to design and construct storage rings for x-ray lithography. Both conventional electromagnets as well as superconducting (SC) dipoles have been incorporated into the various designs. An overview of the worldwide effort to produce commercial x-ray sources will be presented. To better illustrate the elements involved in these sources a closer examination of the Superconducting X-ray Lithography Source Project (SXLS) at BNL will be presented. 11 refs., 1 fig., 5 tabs

  11. Soft X-ray optics

    CERN Document Server

    Spiller, Eberhard A

    1993-01-01

    This text describes optics mainly in the 10 to 500 angstrom wavelength region. These wavelengths are 50 to 100 times shorter than those for visible light and 50 to 100 times longer than the wavelengths of medical x rays or x-ray diffraction from natural crystals. There have been substantial advances during the last 20 years, which one can see as an extension of optical technology to shorter wavelengths or as an extension of x-ray diffraction to longer wavelengths. Artificial diffracting structures like zone plates and multilayer mirrors are replacing the natural crystals of x-ray diffraction.

  12. X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

    This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

  13. X-ray Fluorescence Sectioning

    CERN Document Server

    Cong, Wenxiang

    2012-01-01

    In this paper, we propose an x-ray fluorescence imaging system for elemental analysis. The key idea is what we call "x-ray fluorescence sectioning". Specifically, a slit collimator in front of an x-ray tube is used to shape x-rays into a fan-beam to illuminate a planar section of an object. Then, relevant elements such as gold nanoparticles on the fan-beam plane are excited to generate x-ray fluorescence signals. One or more 2D spectral detectors are placed to face the fan-beam plane and directly measure x-ray fluorescence data. Detector elements are so collimated that each element only sees a unique area element on the fan-beam plane and records the x-ray fluorescence signal accordingly. The measured 2D x-ray fluorescence data can be refined in reference to the attenuation characteristics of the object and the divergence of the beam for accurate elemental mapping. This x-ray fluorescence sectioning system promises fast fluorescence tomographic imaging without a complex inverse procedure. The design can be ad...

  14. X-ray crystallographic studies on C-phycocyanins from cyanobacteria from different habitats: marine and freshwater

    OpenAIRE

    Satyanarayana, L.; Suresh, C. G.; Patel, Anamika; Mishra, Sandhya; Ghosh, Pushpito Kumar

    2005-01-01

    The protein C-phycocyanin, involved in photosynthesis, has been purified from three cyanobacterial species: Spirulina, Phormidium and Lyngbya. These three proteins have been crystallized and characterized using X-ray crystallography.

  15. Radioisotope x-ray analysis

    International Nuclear Information System (INIS)

    Radioisotope x-ray fluorescence and x-ray preferential absorption (XRA) techniques are used extensively for the analysis of materials, covering such diverse applications as analysis of alloys, coal, environmental samples, paper, waste materials, and metalliferous mineral ores and products. Many of these analyses are undertaken in the harsh environment of industrial plants and in the field. Some are continuous on-line analyses of material being processed in industry, where instantaneous analysis information is required for the control of rapidly changing processes. Radioisotope x-ray analysis systems are often tailored to a specific but limited range of applications. They are simpler and often considerably less expensive than analysis systems based on x-ray tubes. These systems are preferred to x-ray tube techniques when simplicity, ruggedness, reliability, and cost of equipment are important; when minimum size, weight, and power consumption are necessary; when a very constant and predictable x-ray output is required; when the use of high-energy x-rays is advantageous; and when short x-ray path lengths are required to minimize the absorption of low-energy x-rays in air. This chapter reviews radioisotope XRF, preferential absorption, and scattering techniques. Some of the basic analysis equations are given. The characteristics of radioisotope sources and x-ray detectors are described, and then the x-ray analytical techniques are presented. The choice of radioisotope technique for a specific application is discussed. This is followed by a summary of applications of these techniques, with a more detailed account given of some of the applications, particularly those of considerable industrial importance. 79 refs., 28 figs., 7 tabs

  16. Micro-crystallography comes of age.

    Science.gov (United States)

    Smith, Janet L; Fischetti, Robert F; Yamamoto, Masaki

    2012-10-01

    The latest revolution in macromolecular crystallography was incited by the development of dedicated, user friendly, micro-crystallography beam lines. Brilliant X-ray beams of diameter 20 μm or less, now available at most synchrotron sources, enable structure determination from samples that previously were inaccessible. Relative to traditional crystallography, crystals with one or more small dimensions have diffraction patterns with vastly improved signal-to-noise when recorded with an appropriately matched beam size. Structures can be solved from isolated, well diffracting regions within inhomogeneous samples. This review summarizes the technological requirements and approaches to producing micro-beams and how they continue to change the practice of crystallography.

  17. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... clothing that might interfere with the x-ray images. Women should always inform their physician and x-ray ... small burst of radiation that passes through the body, recording an image on photographic film or a special detector. Different ...

  18. X-ray diagnostic equipment

    International Nuclear Information System (INIS)

    An X-ray tube is connected to several different image processing devices in X-ray diagnostic equipment. Only a single organ selector is allocated to it, for which the picture parameters for each image processing device are selected. The choice of the correct combination of picture parameters is made by means of a selector switch. (DG)

  19. X-ray tube arrangement

    International Nuclear Information System (INIS)

    An x-ray tube is described incorporating an elongated target/ anode over which the electron beam is deflected and from which x-rays are emitted. Improved methods of monitoring and controlling the amplitude of the beam deflection are presented. (U.K.)

  20. Image reconstruction in serial femtosecond nanocrystallography using x-ray free-electron lasers

    Science.gov (United States)

    Chen, Joe P. J.; Kirian, Richard A.; Beyerlein, Kenneth R.; Bean, Richard J.; Morgan, Andrew J.; Yefanov, Oleksandr M.; Arnal, Romain D.; Wojtas, David H.; Bones, Phil J.; Chapman, Henry N.; Spence, John C. H.; Millane, Rick P.

    2015-09-01

    Serial femtosecond nanocrystallography (SFX) is a form of x-ray coherent diffraction imaging that utilises a stream of tiny nanocrystals of the biological assembly under study, in contrast to the larger crystals used in conventional x-ray crystallography using conventional x-ray synchrotron x-ray sources. Nanocrystallography utilises the extremely brief and intense x-ray pulses that are obtained from an x-ray free-electron laser (XFEL). A key advantage is that some biological macromolecules, such as membrane proteins for example, do not easily form large crystals, but spontaneously form nanocrystals. There is therefore an opportunity for structure determination for biological molecules that are inaccessible using conventional x-ray crystallography. Nanocrystallography introduces a number of interesting image reconstruction problems. Weak diffraction patterns are recorded from hundreds of thousands of nancocrystals in unknown orientations, and these data have to be assembled and merged into a 3D intensity dataset. The diffracted intensities can also be affected by the surface structure of the crystals that can contain incomplete unit cells. Furthermore, the small crystal size means that there is potentially access to diffraction information between the crystalline Bragg peaks. With this information, phase retrieval is possible without resorting to the collection of additional experimental data as is necessary in conventional protein crystallography. We report recent work on the diffraction characteristics of nanocrystals and the resulting reconstruction algorithms.

  1. Interferometric phase detection at x-ray energies via Fano resonance control

    CERN Document Server

    Heeg, K P; Schumacher, D; Wille, H -C; Röhlsberger, R; Pfeifer, T; Evers, J

    2014-01-01

    Modern x-ray light sources promise access to structure and dynamics of matter in largely unexplored spectral regions. However, the desired information is encoded in the light intensity and phase, whereas detectors register only the intensity. This phase problem is ubiquitous in crystallography and imaging, and impedes the exploration of quantum effects at x-ray energies. Here, we demonstrate phase-sensitive measurements characterizing the quantum state of a nuclear two-level system at hard x-ray energies. The nuclei are initially prepared in a superposition state. Subsequently, the relative phase of this superposition is interferometrically reconstructed from the emitted x-rays. Our results form a first step towards x-ray quantum state tomography, and provide new avenues for structure determination and precision metrology via x-ray Fano interference.

  2. Interferometric phase detection at x-ray energies via Fano resonance control.

    Science.gov (United States)

    Heeg, K P; Ott, C; Schumacher, D; Wille, H-C; Röhlsberger, R; Pfeifer, T; Evers, J

    2015-05-22

    Modern x-ray light sources promise access to structure and dynamics of matter in largely unexplored spectral regions. However, the desired information is encoded in the light intensity and phase, whereas detectors register only the intensity. This phase problem is ubiquitous in crystallography and imaging and impedes the exploration of quantum effects at x-ray energies. Here, we demonstrate phase-sensitive measurements characterizing the quantum state of a nuclear two-level system at hard x-ray energies. The nuclei are initially prepared in a superposition state. Subsequently, the relative phase of this superposition is interferometrically reconstructed from the emitted x rays. Our results form a first step towards x-ray quantum state tomography and provide new avenues for structure determination and precision metrology via x-ray Fano interference. PMID:26047250

  3. Semiconductor X-ray detectors

    CERN Document Server

    Lowe, Barrie Glyn

    2014-01-01

    Identifying and measuring the elemental x-rays released when materials are examined with particles (electrons, protons, alpha particles, etc.) or photons (x-rays and gamma rays) is still considered to be the primary analytical technique for routine and non-destructive materials analysis. The Lithium Drifted Silicon (Si(Li)) X-Ray Detector, with its good resolution and peak to background, pioneered this type of analysis on electron microscopes, x-ray fluorescence instruments, and radioactive source- and accelerator-based excitation systems. Although rapid progress in Silicon Drift Detectors (SDDs), Charge Coupled Devices (CCDs), and Compound Semiconductor Detectors, including renewed interest in alternative materials such as CdZnTe and diamond, has made the Si(Li) X-Ray Detector nearly obsolete, the device serves as a useful benchmark and still is used in special instances where its large, sensitive depth is essential. Semiconductor X-Ray Detectors focuses on the history and development of Si(Li) X-Ray Detect...

  4. Multimodal particle size distribution or fractal surface of acrylic acid copolymer nanoparticles: A small-angle X-ray scattering study using direct Fourier and indirect maximum entropy methods

    OpenAIRE

    Mueller, J.J.; Hansen, S; Lukowski, G.; Gast, K.

    1995-01-01

    Acrylic acid copolymers are potential carriers for drug delivery. The surface, surface rugosity and the absolute dimension of the particles are parameters that determine the binding of drugs or detergents, diffusion phenomena at the surface and the distribution of the carrier within the human body. The particle-size distribution and surface rugosity of the particles have been investigated by small-angle X-ray scattering and dynamic light scattering. Direct Fourier transform as well as a new s...

  5. A Newcomer’s Guide to Peptide Crystallography

    OpenAIRE

    Spencer, Ryan K.; Nowick, James S.

    2015-01-01

    Here we provide a guide for adapting the tools developed for protein X-ray crystallography to study the structures and supramolecular assembly of peptides. Peptide crystallography involves selecting a suitable peptide, crystallizing the peptide, collecting X-ray diffraction data, processing the diffraction data, determining the crystallographic phases and generating an electron density map, building and refining models, and depositing the crystallographic structure in the Protein Data Bank (P...

  6. X-ray diffraction apparatus

    International Nuclear Information System (INIS)

    The invention provides an x-ray diffraction apparatus permitting the rotation of the divergence sit in conjunction with the rotation of the x-ray irradiated specimen, whereby the dimensions of the x-ray irradiated portion of the specimen remain substantially constant during the rotation of the specimen. In a preferred embodiment, the divergence slit is connected to a structural element linked with a second structural element connected to the specimen such that the divergence slit rotates at a lower angular speed than the specimen

  7. Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

    Energy Technology Data Exchange (ETDEWEB)

    Van Benschoten, Andrew H. [University of California San Francisco, San Francisco, CA 94158 (United States); Afonine, Pavel V. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Terwilliger, Thomas C.; Wall, Michael E. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Jackson, Colin J. [Australian National University, Canberra, ACT 2601 (Australia); Sauter, Nicholas K. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Adams, Paul D. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); University of California Berkeley, Berkeley, CA 94720 (United States); Urzhumtsev, Alexandre [Institut de Génétique et de Biologie Moléculaire et Cellulaire, CNRS–INSERM–UdS, 1 Rue Laurent Fries, BP 10142, 67404 Illkirch (France); Université de Lorraine, BP 239, 54506 Vandoeuvre-les-Nancy (France); Fraser, James S., E-mail: james.fraser@ucsf.edu [University of California San Francisco, San Francisco, CA 94158 (United States)

    2015-07-28

    A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis.

  8. Liquid sample delivery techniques for serial femtosecond crystallography.

    Science.gov (United States)

    Weierstall, Uwe

    2014-07-17

    X-ray free-electron lasers overcome the problem of radiation damage in protein crystallography and allow structure determination from micro- and nanocrystals at room temperature. To ensure that consecutive X-ray pulses do not probe previously exposed crystals, the sample needs to be replaced with the X-ray repetition rate, which ranges from 120 Hz at warm linac-based free-electron lasers to 1 MHz at superconducting linacs. Liquid injectors are therefore an essential part of a serial femtosecond crystallography experiment at an X-ray free-electron laser. Here, we compare different techniques of injecting microcrystals in solution into the pulsed X-ray beam in vacuum. Sample waste due to mismatch of the liquid flow rate to the X-ray repetition rate can be addressed through various techniques.

  9. Duodenal X-ray diagnostics

    International Nuclear Information System (INIS)

    The publication provides an overview of duodenal X-ray diagnostics with the aid of barium meals in 1362 patients. The introducing paragraphs deal with the topographic anatomy of the region and the methodics of X-ray investigation. The chapter entitled ''processes at the duodenum itself'' describes mainly ulcers, diverticula, congenital anomalies, tumors and inflammations. The neighbourhood processes comprise in the first place diseases having their origin at the pancreas and bile ducts. As a conclusion, endoscopic rectograde cholangio-pancreaticography and percutaneous transhepatic cholangiography are pointed out as advanced X-ray investigation methods. In the annex of X-ray images some of the described phenomena are shown in exemplary manner. (orig./MG)

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... like a photographic negative). Today, most images are digital files that are stored electronically. These stored images ... and places the x-ray film holder or digital recording plate under the table in the area ...

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... pregnant. Many imaging tests are not performed during pregnancy so as not to expose the fetus to ... See the Safety page for more information about pregnancy and x-rays. top of page What does ...

  12. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the baby. See the Safety page for more information about pregnancy and x-rays. top of page ... procedure varies. See the Safety page for more information about radiation dose. Women should always inform their ...

  13. X-ray microtomographic scanners

    Energy Technology Data Exchange (ETDEWEB)

    Syryamkin, V. I., E-mail: klestov-simon@mail.ru; Klestov, S. A., E-mail: klestov-simon@mail.ru [National Research Tomsk State University, Tomsk, 634050 (Russian Federation)

    2015-11-17

    The article studies the operating procedures of an X-ray microtomographic scanner and the module of reconstruction and analysis 3D-image of a test sample in particular. An algorithm for 3D-image reconstruction based on image shadow projections and mathematical methods of the processing are described. Chapter 1 describes the basic principles of X-ray tomography and general procedures of the device developed. Chapters 2 and 3 are devoted to the problem of resources saving by the system during the X-ray tomography procedure, which is achieved by preprocessing of the initial shadow projections. Preprocessing includes background noise removing from the images, which reduces the amount of shadow projections in general and increases the efficiency of the group shadow projections compression. In conclusion, the main applications of X-ray tomography are presented.

  14. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and ... in the typical diagnostic range for this exam. Risks There is always a slight chance of cancer ...

  15. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... can be taken to the patient in a hospital bed or the emergency room. The x-ray ... and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern ...

  16. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the patient in a hospital bed or the emergency room. The x-ray tube is connected to ... equipment is relatively inexpensive and widely available in emergency rooms, physician offices, ambulatory care centers, nursing homes ...

  17. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... or in bones. top of page How should I prepare? Most bone x-rays require no special ... to 10 minutes. top of page What will I experience during and after the procedure? A bone ...

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the body absorb the x-rays in varying degrees. Dense bone absorbs much of the radiation while ... is further reviewed by committees from the American College of Radiology (ACR) and the Radiological Society of ...

  19. Dental X-ray apparatus

    International Nuclear Information System (INIS)

    Intra-oral dental X-ray apparatus for panoramic dental radiography is described in detail. It comprises an electron gun having an elongated tubular target carrier extending into the patient's mouth. The carrier supports an inclined target for direction of an X-ray pattern towards a film positioned externally of the patient's mouth. Image definition is improved by a focusing anode which focuses the electron beam into a sharp spot (0.05 to 0.10 mm diameter) on the target. The potential on the focusing anode is adjustable to vary the size of the spot. An X-ray transmitting ceramic (oxides of Be, Al and Si) window is positioned adjacent to the front face of the target. The electron beam can be magnetically deflected to change the X-ray beam direction. (author)

  20. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... during x-ray examinations to use the lowest radiation dose possible while producing the best images for evaluation. National and international radiology protection organizations continually review and update the technique standards ...

  1. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... technologist, an individual specially trained to perform radiology examinations, positions the patient on the x-ray table ... bone is forming), for comparison purposes. When the examination is complete, you may be asked to wait ...

  2. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... replacement and fracture reductions. look for injury, infection, arthritis , abnormal bone growths and bony changes seen in ... injuries, including fractures, and joint abnormalities, such as arthritis. X-ray equipment is relatively inexpensive and widely ...

  3. X-Ray Assembler Data

    Data.gov (United States)

    U.S. Department of Health & Human Services — Federal regulations require that an assembler who installs one or more certified components of a diagnostic x-ray system submit a report of assembly. This database...

  4. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... a large photographic negative). Today, most images are digital files that are stored electronically. These stored images ... and places the x-ray film holder or digital recording plate under the table in the area ...

  5. Accelerator x-ray sources

    CERN Document Server

    Talman, Richard

    2007-01-01

    This first book to cover in-depth the generation of x-rays in particle accelerators focuses on electron beams produced by means of the novel Energy Recovery Linac (ERL) technology. The resulting highly brilliant x-rays are at the centre of this monograph, which continues where other books on the market stop. Written primarily for general, high energy and radiation physicists, the systematic treatment adopted by the work makes it equally suitable as an advanced textbook for young researchers.

  6. X-ray fluorescence holography

    CERN Document Server

    Hayashi, K; Takahashi, Y

    2003-01-01

    X-ray fluorescence holography (XFH) is a new structural analysis method of determining a 3D atomic arrangement around fluorescing atoms. We developed an XFH apparatus using advanced X-ray techniques and succeeded in obtaining high-quality hologram data. Furthermore, we introduced applications to the structural analysis of a thin film and the environment around dopants and, discussed the quantitative analysis of local lattice distortion. (author)

  7. Electromechanical x-ray generator

    Energy Technology Data Exchange (ETDEWEB)

    Watson, Scott A; Platts, David; Sorensen, Eric B

    2016-05-03

    An electro-mechanical x-ray generator configured to obtain high-energy operation with favorable energy-weight scaling. The electro-mechanical x-ray generator may include a pair of capacitor plates. The capacitor plates may be charged to a predefined voltage and may be separated to generate higher voltages on the order of hundreds of kV in the AK gap. The high voltage may be generated in a vacuum tube.

  8. Nanoflow electrospinning serial femtosecond crystallography

    International Nuclear Information System (INIS)

    A low flow rate liquid microjet method for delivery of hydrated protein crystals to X-ray lasers is presented. Linac Coherent Light Source data demonstrates serial femtosecond protein crystallography with micrograms, a reduction of sample consumption by orders of magnitude. An electrospun liquid microjet has been developed that delivers protein microcrystal suspensions at flow rates of 0.14–3.1 µl min−1 to perform serial femtosecond crystallography (SFX) studies with X-ray lasers. Thermolysin microcrystals flowed at 0.17 µl min−1 and diffracted to beyond 4 Å resolution, producing 14 000 indexable diffraction patterns, or four per second, from 140 µg of protein. Nanoflow electrospinning extends SFX to biological samples that necessitate minimal sample consumption

  9. X-ray Radiation Induces Deprotonation of the Bilin Chromophore in Crystalline D. Radiodurans Phytochrome

    Energy Technology Data Exchange (ETDEWEB)

    Li, Feifei [Brookhaven National Lab. (BNL), Upton, NY (United States); New Mexico State Univ., Las Cruces, NM (United States); Burgie, E. Sethe [Univ. of Wisconsin, Madison, WI (United States); Yu, Tao [Northwestern Univ., Evanston, IL (United States); Heroux, Annie [Brookhaven National Lab. (BNL), Upton, NY (United States); Schatz, George C. [Northwestern Univ., Evanston, IL (United States); Vierstra, Richard D. [Univ. of Wisconsin, Madison, WI (United States); Orville, Allen M. [Brookhaven National Lab. (BNL), Upton, NY (United States)

    2015-02-04

    We report that in the red light-absorbing (Pr) state, the bilin chromophore of the Deinococcus radiodurans proteobacterial phytochrome (DrBphP) is hypersensitive to X-ray photons used in typical synchrotron X-ray protein crystallography experiments. This causes the otherwise fully protonated chromophore to deprotonate without additional major structural changes. Furthermore, these results have major implications for our understanding of the structural and chemical characteristics of the resting and intermediate states of phytochromes and other photoreceptor proteins.

  10. X-ray diagnostic apparatus

    International Nuclear Information System (INIS)

    A falling load type X-ray diagnostic apparatus comprises a low voltage power source, AC-DC converting means connected to the low voltage power source so as to apply a rectified low DC voltage, chopping means connected to the AC-DC converting means and chopping said DC voltage into a low AC voltage, high voltage applying means for transforming said low AC voltage into a high AC voltage, said high AC voltage being applied as a tube voltage to an X-ray tube from which X-rays are irradiated toward an object to be examined, means for controlling a filament heating power of the X-ray tube, programming means for supplying a control signal to said filament heating control means so as to reduce the emission current of said X-ray tube during the irradiation, and chopper control means for controlling the chopping ratio of said chopping means by evaluating said rectified DC voltage with a preset tube voltage generated in said programming means, said programming means compensating said tube voltage by receiving said control signal in such a manner that said tube voltage is maintained substantially constant during the irradiation by varying said preset tube voltage so as to control the chopping ratio based upon the reduction of the filament heating power for the X-ray tube

  11. Low energy (soft) x rays

    International Nuclear Information System (INIS)

    Dosimetry of low-energy (soft) X rays produced by the SOFTEX Model CMBW-2 was performed using Nuclear Associates Type 30 - 330 PTW, Exradin Type A2, and Shonka-Wyckoff ionization chambers with a Keithley Model 602 electrometer. Thermoluminescent (BeO chip) dosimeters were used with a Harshaw Detector 2000-A and Picoammeter-B readout system. Beam quality measurements were made using aluminum absorbers; exposure rates were assessed by the current of the X-ray tube and by exposure times. Dose distributions were established, and the average factors for non-uniformity were calculated. The means of obtaining accurate absorbed and exposed doses using these methods are discussed. Survival of V79 cells was assessed by irradiating them with soft X rays, 200 kVp X rays, and 60Co gamma rays. The relative biological effectiveness (RBE) values for soft X rays with 0, 0.2, 0.7 mm added thicknesses of aluminum were 1.6, which were compared to 60Co. The RBE of 200 kVp X rays relative to 60Co was 1.3. Results of this study are available for reference in future RERF studies of cell survival. (author)

  12. Center for X-Ray Optics, 1992

    International Nuclear Information System (INIS)

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors

  13. Nanoflow electrospinning serial femtosecond crystallography.

    Science.gov (United States)

    Sierra, Raymond G; Laksmono, Hartawan; Kern, Jan; Tran, Rosalie; Hattne, Johan; Alonso-Mori, Roberto; Lassalle-Kaiser, Benedikt; Glöckner, Carina; Hellmich, Julia; Schafer, Donald W; Echols, Nathaniel; Gildea, Richard J; Grosse-Kunstleve, Ralf W; Sellberg, Jonas; McQueen, Trevor A; Fry, Alan R; Messerschmidt, Marc M; Miahnahri, Alan; Seibert, M Marvin; Hampton, Christina Y; Starodub, Dmitri; Loh, N Duane; Sokaras, Dimosthenis; Weng, Tsu-Chien; Zwart, Petrus H; Glatzel, Pieter; Milathianaki, Despina; White, William E; Adams, Paul D; Williams, Garth J; Boutet, Sébastien; Zouni, Athina; Messinger, Johannes; Sauter, Nicholas K; Bergmann, Uwe; Yano, Junko; Yachandra, Vittal K; Bogan, Michael J

    2012-11-01

    An electrospun liquid microjet has been developed that delivers protein microcrystal suspensions at flow rates of 0.14-3.1 µl min(-1) to perform serial femtosecond crystallography (SFX) studies with X-ray lasers. Thermolysin microcrystals flowed at 0.17 µl min(-1) and diffracted to beyond 4 Å resolution, producing 14,000 indexable diffraction patterns, or four per second, from 140 µg of protein. Nanoflow electrospinning extends SFX to biological samples that necessitate minimal sample consumption. PMID:23090408

  14. Warm dense crystallography

    Science.gov (United States)

    Valenza, Ryan A.; Seidler, Gerald T.

    2016-03-01

    The intense femtosecond-scale pulses from x-ray free electron lasers (XFELs) are able to create and interrogate interesting states of matter characterized by long-lived nonequilibrium semicore or core electron occupancies or by the heating of dense phases via the relaxation cascade initiated by the photoelectric effect. We address here the latter case of "warm dense matter" (WDM) and investigate the observable consequences of x-ray heating of the electronic degrees of freedom in crystalline systems. We report temperature-dependent density functional theory calculations for the x-ray diffraction from crystalline LiF, graphite, diamond, and Be. We find testable, strong signatures of condensed-phase effects that emphasize the importance of wide-angle scattering to study nonequilibrium states. These results also suggest that the reorganization of the valence electron density at eV-scale temperatures presents a confounding factor to achieving atomic resolution in macromolecular serial femtosecond crystallography (SFX) studies at XFELs, as performed under the "diffract before destroy" paradigm.

  15. Preparation, crystallization and preliminary X-ray diffraction analysis of two intestinal fatty-acid binding proteins in the presence of 11-(dansylamino)undecanoic acid

    International Nuclear Information System (INIS)

    Intestinal fatty-acid binding proteins from human and rat have been crystallized in complex with the fluorescent probe 11-(dansylamino)undecanoic acid. Diffraction data for the crystals were collected to 1.8 Å resolution (human) and 1.6 Å resolution (rat). Fatty-acid binding proteins (FABPs) are abundantly expressed proteins that bind a range of lipophilic molecules. They have been implicated in the import and intracellular distribution of their ligands and have been linked with metabolic and inflammatory responses in the cells in which they are expressed. Despite their high sequence identity, human intestinal FABP (hIFABP) and rat intestinal FABP (rIFABP) bind some ligands with different affinities. In order to address the structural basis of this differential binding, diffraction-quality crystals have been obtained of hIFABP and rIFABP in complex with the fluorescent fatty-acid analogue 11-(dansylamino)undecanoic acid

  16. The Coherent X-ray Imaging instrument at the Linac Coherent Light Source

    Energy Technology Data Exchange (ETDEWEB)

    Liang, Mengning; Williams, Garth J.; Messerschmidt, Marc; Seibert, M. Marvin; Montanez, Paul A.; Hayes, Matt; Milathianaki, Despina; Aquila, Andrew; Hunter, Mark S.; Koglin, Jason E.; Schafer, Donald W.; Guillet, Serge; Busse, Armin; Bergan, Robert; Olson, William; Fox, Kay; Stewart, Nathaniel; Curtis, Robin; Miahnahri, Alireza Alan; Boutet, Sébastien, E-mail: sboutet@slac.stanford.edu [Linac Coherent Light Source, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, CA 94025 (United States)

    2015-04-15

    Description of the Coherent X-ray Imaging (CXI) instrument at the Linac Coherent Light Source. Recent scientific highlights illustrate the femtosecond crystallography, high power density and extreme matter capabilities of the CXI instrument. The Coherent X-ray Imaging (CXI) instrument specializes in hard X-ray, in-vacuum, high power density experiments in all areas of science. Two main sample chambers, one containing a 100 nm focus and one a 1 µm focus, are available, each with multiple diagnostics, sample injection, pump–probe and detector capabilities. The flexibility of CXI has enabled it to host a diverse range of experiments, from biological to extreme matter.

  17. X-ray Echo Spectroscopy

    Science.gov (United States)

    Shvyd'ko, Yuri

    2016-02-01

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >108 ) with broadband ≃5 - 13 meV dispersing systems are introduced featuring more than 103 signal enhancement. The technique is general, applicable in different photon frequency domains.

  18. X-ray echo spectroscopy

    CERN Document Server

    Shvyd'ko, Yuri

    2015-01-01

    X-ray echo spectroscopy, a counterpart of neutron spin-echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a point-like x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x-rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1--0.02-meV ultra-high-resolution IXS applications (resolving power $> 10^8$) with broadband $\\simeq$~5--13~meV dispersing systems are introduced featuring more than $10^3$ signal e...

  19. X-ray Echo Spectroscopy.

    Science.gov (United States)

    Shvyd'ko, Yuri

    2016-02-26

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >10^{8}) with broadband ≃5-13  meV dispersing systems are introduced featuring more than 10^{3} signal enhancement. The technique is general, applicable in different photon frequency domains.

  20. Dental X-ray apparatus

    International Nuclear Information System (INIS)

    Intra-oral X-ray apparatus which reduces the number of exposures necessary to obtain panoramic dental radiographs is described in detail. It comprises an electron gun, a tubular target carrier projecting from the gun along the beam axis and carrying at its distal end a target surrounded by a shield of X-ray opaque material. This shield extends forward and laterally of the target and has surfaces which define a wedge or cone-shaped radiation pattern delimited vertically by the root tips of the patient's teeth. A film holder is located externally of the patient's mouth. A disposable member can fit on the target carrier to depress the patient's tongue out of the radiation pattern and to further shield the roof of the mouth. The electron beam can be magnetically deflected to change the X-ray beam direction. (author)

  1. X-ray imaging: Perovskites target X-ray detection

    Science.gov (United States)

    Heiss, Wolfgang; Brabec, Christoph

    2016-05-01

    Single crystals of perovskites are currently of interest to help fathom fundamental physical parameters limiting the performance of perovskite-based polycrystalline solar cells. Now, such perovskites offer a technology platform for optoelectronic devices, such as cheap and sensitive X-ray detectors.

  2. High-resolution X-ray study of the effects of deuteration on crystal growth and the crystal structure of proteinase K.

    Science.gov (United States)

    Chatake, Toshiyuki; Ishikawa, Takuya; Yanagisawa, Yasuhide; Yamada, Taro; Tanaka, Ichiro; Fujiwara, Satoru; Morimoro, Yukio

    2011-11-01

    Deuteration of macromolecules is an important technique in neutron protein crystallography. Solvent deuteration of protein crystals is carried out by replacing water (H(2)O) with heavy water (D(2)O) prior to neutron diffraction experiments in order to diminish background noise. The effects of solvent deuteration on the crystallization of proteinase K (PK) with polyethylene glycol as a precipitant were investigated using high-resolution X-ray crystallography. In previous studies, eight NO(3)(-) anions were included in the PK crystal unit cell grown in NaNO(3) solution. In this study, however, the PK crystal structure did not contain NO(3)(-) anions; consequently, distortions of amino acids arising from the presence of NO(3)(-) anions were avoided in the present crystal structures. High-resolution (1.1 Å) X-ray diffraction studies showed that the degradation of PK crystals induced by solvent deuteration was so small that this degradation would be negligible for the purpose of neutron protein crystallography experiments at medium resolution. Comparison of the nonhydrogen structures of nondeuterated and deuterated crystal structures demonstrated very small structural differences. Moreover, a positive correlation between the root-mean-squared differences and B factors indicated that no systematic difference existed.

  3. X-ray hot plasma diagnostics

    International Nuclear Information System (INIS)

    X-ray plasma emission study is powerful diagnostic tool of hot plasmas. In this review article the main techniques of X-ray plasma emission measurement are shortly presented: X-ray spectrometry using absorbent filters, crystal and grating spectrometers, imaging techniques using pinhole cameras, X-ray microscopes and Fresnel zone plate cameras, X-ray plasma emission calorimetry. Advances in these techniques with examples for different hot plasma devices are also presentes. (author)

  4. Towards phasing using high X-ray intensity

    Directory of Open Access Journals (Sweden)

    Lorenzo Galli

    2015-11-01

    Full Text Available X-ray free-electron lasers (XFELs show great promise for macromolecular structure determination from sub-micrometre-sized crystals, using the emerging method of serial femtosecond crystallography. The extreme brightness of the XFEL radiation can multiply ionize most, if not all, atoms in a protein, causing their scattering factors to change during the pulse, with a preferential `bleaching' of heavy atoms. This paper investigates the effects of electronic damage on experimental data collected from a Gd derivative of lysozyme microcrystals at different X-ray intensities, and the degree of ionization of Gd atoms is quantified from phased difference Fourier maps. A pattern sorting scheme is proposed to maximize the ionization contrast and the way in which the local electronic damage can be used for a new experimental phasing method is discussed.

  5. Towards phasing using high X-ray intensity.

    Science.gov (United States)

    Galli, Lorenzo; Son, Sang-Kil; Barends, Thomas R M; White, Thomas A; Barty, Anton; Botha, Sabine; Boutet, Sébastien; Caleman, Carl; Doak, R Bruce; Nanao, Max H; Nass, Karol; Shoeman, Robert L; Timneanu, Nicusor; Santra, Robin; Schlichting, Ilme; Chapman, Henry N

    2015-11-01

    X-ray free-electron lasers (XFELs) show great promise for macromolecular structure determination from sub-micrometre-sized crystals, using the emerging method of serial femtosecond crystallography. The extreme brightness of the XFEL radiation can multiply ionize most, if not all, atoms in a protein, causing their scattering factors to change during the pulse, with a preferential 'bleaching' of heavy atoms. This paper investigates the effects of electronic damage on experimental data collected from a Gd derivative of lysozyme microcrystals at different X-ray intensities, and the degree of ionization of Gd atoms is quantified from phased difference Fourier maps. A pattern sorting scheme is proposed to maximize the ionization contrast and the way in which the local electronic damage can be used for a new experimental phasing method is discussed. PMID:26594370

  6. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    Directory of Open Access Journals (Sweden)

    Robert M. Lawrence

    2015-07-01

    Full Text Available Serial femtosecond crystallography (SFX using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ∼700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ∼40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is an important step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  7. X-Ray Solution Scattering Study of Four Escherichia coli Enzymes Involved in Stationary-Phase Metabolism.

    Directory of Open Access Journals (Sweden)

    Liubov A Dadinova

    Full Text Available The structural analyses of four metabolic enzymes that maintain and regulate the stationary growth phase of Escherichia coli have been performed primarily drawing on the results obtained from solution small angle X-ray scattering (SAXS and other structural techniques. The proteins are (i class I fructose-1,6-bisphosphate aldolase (FbaB; (ii inorganic pyrophosphatase (PPase; (iii 5-keto-4-deoxyuronate isomerase (KduI; and (iv glutamate decarboxylase (GadA. The enzyme FbaB, that until now had an unknown structure, is predicted to fold into a TIM-barrel motif that form globular protomers which SAXS experiments show associate into decameric assemblies. In agreement with previously reported crystal structures, PPase forms hexamers in solution that are similar to the previously reported X-ray crystal structure. Both KduI and GadA that are responsible for carbohydrate (pectin metabolism and acid stress responses, respectively, form polydisperse mixtures consisting of different oligomeric states. Overall the SAXS experiments yield additional insights into shape and organization of these metabolic enzymes and further demonstrate the utility of hybrid methods, i.e., solution SAXS combined with X-ray crystallography, bioinformatics and predictive 3D-structural modeling, as tools to enrich structural studies. The results highlight the structural complexity that the protein components of metabolic networks may adopt which cannot be fully captured using individual structural biology techniques.

  8. X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    The seventh edition of Philips' Review of Literature on x-ray fluorescence spectrometry starts with a list of conference proceedings on the subject, organised by the Philips organisation at regular intervals in various European countries. It is followed by a list of bulletins. The bibliography is subdivided according to spectra, equipment, applications and absorption analysis

  9. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Images related to X-ray (Radiography) - Bone About this Site RadiologyInfo.org is produced by: Please note ... you can search the ACR-accredited facilities database . This website does not provide cost information. The costs ...

  10. X-ray backscatter imaging

    Science.gov (United States)

    Dinca, Dan-Cristian; Schubert, Jeffrey R.; Callerame, J.

    2008-04-01

    In contrast to transmission X-ray imaging systems where inspected objects must pass between source and detector, Compton backscatter imaging allows both the illuminating source as well as the X-ray detector to be on the same side of the target object, enabling the inspection to occur rapidly and in a wide variety of space-constrained situations. A Compton backscatter image is similar to a photograph of the contents of a closed container, taken through the container walls, and highlights low atomic number materials such as explosives, drugs, and alcohol, which appear as especially bright objects by virtue of their scattering characteristics. Techniques for producing X-ray images based on Compton scattering will be discussed, along with examples of how these systems are used for both novel security applications and for the detection of contraband materials at ports and borders. Differences between transmission and backscatter images will also be highlighted. In addition, tradeoffs between Compton backscatter image quality and scan speed, effective penetration, and X-ray source specifications will be discussed.

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available Toggle navigation Test/Treatment Patient Type Screening/Wellness Disease/Condition Safety En Español More Info Images/Videos News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone ...

  12. X-Ray Diffractive Optics

    Science.gov (United States)

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

    X-ray optics were fabricated with the capability of imaging solar x-ray sources with better than 0.1 arcsecond angular resolution, over an order of magnitude finer than is currently possible. Such images would provide a new window into the little-understood energy release and particle acceleration regions in solar flares. They constitute one of the most promising ways to probe these regions in the solar atmosphere with the sensitivity and angular resolution needed to better understand the physical processes involved. A circular slit structure with widths as fine as 0.85 micron etched in a silicon wafer 8 microns thick forms a phase zone plate version of a Fresnel lens capable of focusing approx. =.6 keV x-rays. The focal length of the 3-cm diameter lenses is 100 microns, and the angular resolution capability is better than 0.1 arcsecond. Such phase zone plates were fabricated in Goddard fs Detector Development Lab. (DDL) and tested at the Goddard 600-microns x-ray test facility. The test data verified that the desired angular resolution and throughput efficiency were achieved.

  13. X-ray film processing

    International Nuclear Information System (INIS)

    X-ray films have to be highly sensitive, for radiation protection reasons. The films used in radiology are coated on both sides with a photosensitive emulsion. This applies to all dental films. Their properties and the development of the different exposed films are explained. (DG)

  14. X-rays and magnetism.

    Science.gov (United States)

    Fischer, Peter; Ohldag, Hendrik

    2015-09-01

    Magnetism is among the most active and attractive areas in modern solid state physics because of intriguing phenomena interesting to fundamental research and a manifold of technological applications. State-of-the-art synthesis of advanced magnetic materials, e.g. in hybrid structures paves the way to new functionalities. To characterize modern magnetic materials and the associated magnetic phenomena, polarized x-rays have emerged as unique probes due to their specific interaction with magnetic materials. A large variety of spectroscopic and microscopic techniques have been developed to quantify in an element, valence and site-sensitive way properties of ferro-, ferri-, and antiferromagnetic systems, such as spin and orbital moments, and to image nanoscale spin textures and their dynamics with sub-ns time and almost 10 nm spatial resolution. The enormous intensity of x-rays and their degree of coherence at next generation x-ray facilities will open the fsec time window to magnetic studies addressing fundamental time scales in magnetism with nanometer spatial resolution. This review will give an introduction into contemporary topics of nanoscale magnetic materials and provide an overview of analytical spectroscopy and microscopy tools based on x-ray dichroism effects. Selected examples of current research will demonstrate the potential and future directions of these techniques.

  15. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... over time. top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... cancer from excessive exposure to radiation. However, the benefit of an accurate diagnosis far outweighs the risk. ...

  16. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... over time. top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology ...

  17. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... for more information about pregnancy and x-rays. A Word About Minimizing Radiation Exposure Special care is ... encourage linking to this site. × Recommend RadiologyInfo to a friend Send to (friend's e-mail address): From ( ...

  18. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    OpenAIRE

    de Groot, F. M. F.

    2001-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption process. Section II discusses 1s X-ray absorption, i.e., the K edges, and section III deals with 2p X-ray absorption, the L edges. X-ray emission is discussed in, respectively, the L edges. X-ray emis...

  19. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    NARCIS (Netherlands)

    Groot, F.M.F. de

    2001-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption pro

  20. An Exercise in X-Ray Diffraction Using the Polymorphic Transition of Nickel Chromite.

    Science.gov (United States)

    Chipman, David W.

    1980-01-01

    Describes a laboratory experiment appropriate for a course in either x-ray crystallography or mineralogy. The experiment permits the direct observation of a polymorphic transition in nickel chromite without the use of a special heating stage or heating camera. (Author/GS)

  1. Simultaneous X-ray diffraction from multiple single crystals of macromolecules

    DEFF Research Database (Denmark)

    Paithankar, Karthik S.; Sørensen, Henning Osholm; Wright, Jonathan P.;

    2011-01-01

    The potential in macromolecular crystallography for using multiple crystals to collect X-ray diffraction data simultaneously from assemblies of up to seven crystals is explored. The basic features of the algorithms used to extract data and their practical implementation are described. The procedu...

  2. Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; Kick, Leonhard M.; Gati, Cornelius; Nelson, Garrett; Deupi, Xavier; Standfuss, Jörg; Schertler, Gebhard; Panneels, Valérie, E-mail: valerie.panneels@psi.ch [Paul Scherrer Institute, OFLC/103, 5232 Villigen-PSI (Switzerland)

    2015-06-27

    A new batch preparation method is presented for high-density micrometre-sized crystals of the G protein-coupled receptor rhodopsin for use in time-resolved serial femtosecond crystallography at an X-ray free-electron laser using a liquid jet. Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.

  3. An introduction to three-dimensional X-ray diffraction microscopy

    DEFF Research Database (Denmark)

    Poulsen, Henning Friis

    2012-01-01

    Three-dimensional X-ray diffraction microscopy is a fast and nondestructive structural characterization technique aimed at studies of the individual crystalline elements (grains or subgrains) within millimetre-sized polycrystalline specimens. It is based on two principles: the use of highly penet....... © 2012 International Union of Crystallography Printed in Singapore-all rights reserved....

  4. Membrane protein structural biology using X-ray free electron lasers.

    Science.gov (United States)

    Neutze, Richard; Brändén, Gisela; Schertler, Gebhard F X

    2015-08-01

    Membrane protein structural biology has benefitted tremendously from access to micro-focus crystallography at synchrotron radiation sources. X-ray free electron lasers (XFELs) are linear accelerator driven X-ray sources that deliver a jump in peak X-ray brilliance of nine orders of magnitude and represent a disruptive technology with potential to dramatically change the field. Membrane proteins were amongst the first macromolecules to be studied with XFEL radiation and include proof-of-principle demonstrations of serial femtosecond crystallography (SFX), the observation that XFEL data can deliver damage free crystallographic structures, initial experiments towards recording structural information from 2D arrays of membrane proteins, and time-resolved SFX, time-resolved wide angle X-ray scattering and time-resolved X-ray emission spectroscopy studies. Conversely, serial crystallography methods are now being applied using synchrotron radiation. We believe that a context dependent choice of synchrotron or XFEL radiation will accelerate progress towards novel insights in understanding membrane protein structure and dynamics.

  5. Microscale X-ray Absorption Spectroscopy on the GSECARS Sector 13 at the APS

    CERN Document Server

    Stephen-Sutto

    2000-01-01

    GeoSoilEnviroCARS (GSECARS) is a national user facility for frontier research in the earth sciences using synchrotrons radiation at the Advanced Photon Source, Argonne National Laboratory. GSECARS provides earth scientists with access to the high-brilliance hard x-rays from this third-generation synchrotrons light source. The research conducted at this facility will advance our knowledge of the composition, structure and properties of earth materials, the processes they control and the processes that produce them. All principal synchrotron-based analytical techniques in demand by earth scientists are being brought to bear on earth science problems: (1) high-pressure/high-temperature crystallography and spectroscopy using the diamond anvil cell; (2) high-pressure/high-temperature crystallography using the large-volume press; (3) powder, single crystal and interface diffraction; (4) x-ray absorption fine structure (XAFS) spectroscopy; (5) x-ray fluorescence microprobe analysis and microspectroscopy; and (6) mic...

  6. The effects of X-ray irradiation on the induction of α-amylase synthesis by gibberelic acid in the aleurone system of barley

    International Nuclear Information System (INIS)

    The influence of ionizing radiation on a system without DNA replication and cell division was investigated with the aid of GA3-induced α-amylase synthesis in aleurone cells of barley. The reaction of the system was determined by dose effect curves (after irradiation of one half of the endosperms in rest) for the synthesis and secretion of α-amylase, protein, and reducing sugars. The system proves to be highly radiation-resistant. The course of the synthesis of α-amylase after X-ray irradiation with varying doses during enzyme synthesis suggests that transcription occurs in the middle of the lag-phase and is the most sensitive stage in enzyme synthesis, while translation alone is less sensitive to radiation. (BSC/AK)

  7. (R,R-Tartaric Acid Dimethyl Diester from X-Ray and Ab Initio Studies: Factors Influencing Its Conformation and Packing

    Directory of Open Access Journals (Sweden)

    J. Rychlewski

    1997-07-01

    Full Text Available The conformation of dimethyl (R,R-tartrate has been analyzed on the basis of the single crystal X-ray diffraction method as well as by ab-initio quantum chemical studies. The results showed that the extended T conformation containing two planar hydroxyester moieties predominates in both ab-initio and X-ray studies. The lowest energy conformer in ab-initio calculations has C2 symmetry and hydrogen bonds between a hydroxyl group and the nearest carbonyl oxygen. The second in energetical sequence, with an energy difference of only 1.2 kcal/mol, is the asymmetrical conformer, which differs from the lowest energy form by the rotation of one of the ester groups by 180°. Intramolecular OH...O hydrogen bonds observed in this rotamer again involve only proximal functional groups. This conformer is present in the crystal structure of the studied compound, although its conformation in the solid state is no longer stabilized by intramolecular hydrogen bonds of the type mentioned above. In the crystal, hydroxyl groups are mostly involved in intermolecular hydrogen bonds and form only a weak intramolecular hydrogen bond with each other. The planar arrangement of the α-hydroxyester moieties combined with the extended conformation of the carbon chain seems to be stabilized by the intramolecular hydrogen bonds between neighboring functional groups and by the long range dipole-dipole interactions between two pairs of CO and (βC-H bonds.

  8. Electron crystallography of ultrathin 3D protein crystals: atomic model with charges.

    Science.gov (United States)

    Yonekura, Koji; Kato, Kazuyuki; Ogasawara, Mitsuo; Tomita, Masahiro; Toyoshima, Chikashi

    2015-03-17

    Membrane proteins and macromolecular complexes often yield crystals too small or too thin for even the modern synchrotron X-ray beam. Electron crystallography could provide a powerful means for structure determination with such undersized crystals, as protein atoms diffract electrons four to five orders of magnitude more strongly than they do X-rays. Furthermore, as electron crystallography yields Coulomb potential maps rather than electron density maps, it could provide a unique method to visualize the charged states of amino acid residues and metals. Here we describe an attempt to develop a methodology for electron crystallography of ultrathin (only a few layers thick) 3D protein crystals and present the Coulomb potential maps at 3.4-Å and 3.2-Å resolution, respectively, obtained from Ca(2+)-ATPase and catalase crystals. These maps demonstrate that it is indeed possible to build atomic models from such crystals and even to determine the charged states of amino acid residues in the Ca(2+)-binding sites of Ca(2+)-ATPase and that of the iron atom in the heme in catalase.

  9. Center for X-Ray Optics, 1986

    International Nuclear Information System (INIS)

    The Center for X-Ray Optics has made substantial progress during the past year on the development of very high resolution x-ray technologies, the generation of coherent radiation at x-ray wavelengths, and, based on these new developments, had embarked on several scientific investigations that would not otherwise have been possible. The investigations covered in this report are topics on x-ray sources, x-ray imaging and applications, soft x-ray spectroscopy, synchrotron radiation, advanced light source and magnet structures for undulators and wigglers

  10. Soft x-ray tomoholography

    International Nuclear Information System (INIS)

    We demonstrate an x-ray imaging method that combines Fourier transform holography with tomography (‘tomoholography’) for three-dimensional (3D) microscopic imaging. A 3D image of a diatom shell with a spatial resolution of 140 nm is presented. The experiment is realized by using a small gold sphere as the reference wave source for holographic imaging. This setup allows us to rotate the sample and to collect a number of 2D projections for tomography. (paper)

  11. Soft x-ray tomoholography

    OpenAIRE

    Guehrs, E.; Stadler, A.M.; Flewett, S.; Frömmel, S.; Geilhufe, J.; Pfau, B; Rander, T.; Schaffert, S.; Büldt, G; Eisebitt, S.

    2012-01-01

    We demonstrate an x-ray imaging method that combines Fourier transform holography with tomography ('tomoholography') for three-dimensional (3D) microscopic imaging. A 3D image of a diatom shell with a spatial resolution of 140 nm is presented. The experiment is realized by using a small gold sphere as the reference wave source for holographic imaging. This setup allows us to rotate the sample and to collect a number of 2D projections for tomography.

  12. X-ray tube arrangements

    International Nuclear Information System (INIS)

    A technique for ensuring the rapid correction of both amplitude and offset errors in the deflectional movement of an electron beam along an X-ray emissive target is described. The movement is monitored at at least two positions during a sweep and differences, between the two movements and a desired movement, at these positions are combined in different proportions to produce a corrective servo signal. Such arrangements find application, for example, in computerised tomographic scanners. (author)

  13. X-ray-powered macronovae

    CERN Document Server

    Kisaka, Shota; Nakar, Ehud

    2015-01-01

    A macronova (or kilonova) was observed as an infrared excess several days after short gamma-ray burst, GRB 130603B. Although the $r$-process radioactivity is widely discussed as an energy source, it requires huge mass of ejecta from a neutron star (NS) binary merger. We propose that the X-ray excess simultaneously observed with the infrared excess can naturally heat the ejecta, leading to the thermal re-emission as observed in infrared. This X-ray-powered model explains both the X-ray and infrared excesses with a single energy source by the central engine like a black hole, and allows for broader parameter region, in particular smaller ejecta mass $\\sim10^{-3}-10^{-2}M_{\\odot}$ with iron mixed as suggested by general relativistic simulations for typical NS-NS mergers, than the previous models. We also discuss the other macronova candidates in GRB 060614 and GRB 080503, and implications for the search of electromagnetic counterparts to gravitational waves.

  14. X-Ray-powered Macronovae

    Science.gov (United States)

    Kisaka, Shota; Ioka, Kunihito; Nakar, Ehud

    2016-02-01

    A macronova (or kilonova) was observed as an infrared excess several days after the short gamma-ray burst GRB 130603B. Although the r-process radioactivity is widely discussed as an energy source, it requires a huge mass of ejecta from a neutron star (NS) binary merger. We propose a new model in which the X-ray excess gives rise to the simultaneously observed infrared excess via thermal re-emission, and explore what constraints this would place on the mass and velocity of the ejecta. This X-ray-powered model explains both the X-ray and infrared excesses with a single energy source such as the central engine like a black hole, and allows for a broader parameter region than the previous models, in particular a smaller ejecta mass ˜ {10}-3{--}{10}-2{M}⊙ and higher iron abundance mixed as suggested by general relativistic simulations for typical NS-NS mergers. We also discuss the other macronova candidates in GRB 060614 and GRB 080503, and the implications for the search of electromagnetic counterparts to gravitational waves.

  15. CCD sensors in synchrotron X-ray detectors

    Science.gov (United States)

    Strauss, M. G.; Naday, I.; Sherman, I. S.; Kraimer, M. R.; Westbrook, E. M.; Zaluzec, N. J.

    1988-04-01

    The intense photon flux from advanced synchrotron light sources, such as the 7-GeV synchrotron being designed at Argonne, require integrating-type detectors. Charge-coupled devices (CCDs) are well suited as synchrotron X-ray detectors. When irradiated indirectly via a phosphor followed by reducing optics, diffraction patterns of 100 cm 2 can be imaged on a 2 cm 2 CCD. With a conversion efficiency of ˜ 1 CCD electron/X-ray photon, a peak saturation capacity of > 10 6 X-rays can be obtained. A programmable CCD controller operating at a clock frequency of 20 MHz has been developed. The readout rate is 5 × 10 6 pixels/s and the shift rate in the parallel registers is 10 6 lines/s. The test detector was evaluated in two experiments. In protein crystallography diffraction patterns have been obtained from a lysozyme crystal using a conventional rotating anode X-ray generator. Based on these results we expect to obtain at a synchrotron diffraction images at a rate of ˜ 1 frame/s or a complete 3-dimensional data set from a single crystal in ˜ 2 min. In electron energy-loss spectroscopy (EELS), the CCD was used in a parallel detection mode which is similar to the mode array detectors are used in dispersive EXAFS. With a beam current corresponding to 3 × 10 9 electron/s on the detector, a series of 64 spectra were recorded on the CCD in a continuous sequence without interruption due to readout. The frame-to-frame pixel signal fluctuations had σ = 0.4% from which DQE = 0.4 was obtained, where the detector conversion efficiency was 2.6 CCD electrons/X-ray photon. These multiple frame series also showed the time-resolved modulation of the electron microscope optics by stray magnetic fields.

  16. "Newton's cradle" proton relay with amide-imidic acid tautomerization in inverting cellulase visualized by neutron crystallography.

    Science.gov (United States)

    Nakamura, Akihiko; Ishida, Takuya; Kusaka, Katsuhiro; Yamada, Taro; Fushinobu, Shinya; Tanaka, Ichiro; Kaneko, Satoshi; Ohta, Kazunori; Tanaka, Hiroaki; Inaka, Koji; Higuchi, Yoshiki; Niimura, Nobuo; Samejima, Masahiro; Igarashi, Kiyohiko

    2015-08-01

    Hydrolysis of carbohydrates is a major bioreaction in nature, catalyzed by glycoside hydrolases (GHs). We used neutron diffraction and high-resolution x-ray diffraction analyses to investigate the hydrogen bond network in inverting cellulase PcCel45A, which is an endoglucanase belonging to subfamily C of GH family 45, isolated from the basidiomycete Phanerochaete chrysosporium. Examination of the enzyme and enzyme-ligand structures indicates a key role of multiple tautomerizations of asparagine residues and peptide bonds, which are finally connected to the other catalytic residue via typical side-chain hydrogen bonds, in forming the "Newton's cradle"-like proton relay pathway of the catalytic cycle. Amide-imidic acid tautomerization of asparagine has not been taken into account in recent molecular dynamics simulations of not only cellulases but also general enzyme catalysis, and it may be necessary to reconsider our interpretation of many enzymatic reactions. PMID:26601228

  17. Aspergillosis - chest x-ray (image)

    Science.gov (United States)

    ... usually occurs in immunocompromised individuals. Here, a chest x-ray shows that the fungus has invaded the lung ... are usually seen as black areas on an x-ray. The cloudiness on the left side of this ...

  18. Stabilized x-ray generator power supply

    International Nuclear Information System (INIS)

    X-ray diffraction and X-ray fluorescence analysis are very much adopted in laboratories to determine the type and structure of the constituent compounds in solid materials, chemical composition of materials, stress developed on metals etc. These experiments need X-ray beam of fixed intensity and wave length. This can only be achieved by X-ray generator having highly stabilized tube voltage and tube current. This paper describes how X-ray tube high voltage and electron beam current are stabilized. This paper also highlights generation of X-rays, diffractometry and X-ray fluorescence analysis and their wide applications. Principle of operation for stabilizing the X-ray tube voltage and current, different protection circuits adopted, special features of the mains H.V. transformer and H.T. tank are described in this report. (author)

  19. Neutron protein crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Niimura, Nobuo [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment

    1998-10-01

    X-ray diffraction of single crystal has enriched the knowledge of various biological molecules such as proteins, DNA, t-RNA, viruses, etc. It is difficult to make structural analysis of hydrogen atoms in a protein using X-ray crystallography, whereas neutron diffraction seems usable to directly determine the location of those hydrogen atoms. Here, neutron diffraction method was applied to structural analysis of hen egg-white lysozyme. Since the crystal size of a protein to analyze is generally small (5 mm{sup 3} at most), the neutron beam at the sample position in monochromator system was set to less than 5 x 5 mm{sup 2} and beam divergence to 0.4 degree or less. Neutron imaging plate with {sup 6}Li or Gd mixed with photostimulated luminescence material was used and about 2500 Bragg reflections were recorded in one crystal setting. A total of 38278 reflections for 2.0 A resolution were collected in less than 10 days. Thus, stereo views of Trp-111 omit map around the indol ring of Trp-111 was presented and the three-dimensional arrangement of 696H and 264D atoms in the lysozyme molecules was determined using the omit map. (M.N.)

  20. Phase-sensitive X-ray imager

    Science.gov (United States)

    Baker, Kevin Louis

    2013-01-08

    X-ray phase sensitive wave-front sensor techniques are detailed that are capable of measuring the entire two-dimensional x-ray electric field, both the amplitude and phase, with a single measurement. These Hartmann sensing and 2-D Shear interferometry wave-front sensors do not require a temporally coherent source and are therefore compatible with x-ray tubes and also with laser-produced or x-pinch x-ray sources.

  1. Optical element for X-ray microscopy

    OpenAIRE

    Chadzitaskos, G.

    2008-01-01

    We present a proposal for a X-ray optical element suitable for X-ray microscopy and other X-ray-based display systems. Its principle is based on the Fresnel lenses condition and the Bragg condition for X-ray scattering on a slice of monocrystal. These conditions are fulfilled simultaneously due to a properly machined shape of the monocrystal with a stress at its ends.

  2. Time-resolved and in-situ X-ray scattering methods beyond photoactivation: Utilizing high-flux X-ray sources for the study of ubiquitous non-photoactive proteins.

    Science.gov (United States)

    Jain, Rohit; Techert, Simone

    2016-01-01

    X-ray scattering technique, comprising of small-angle/wide-angle X-ray scattering (SAXS/WAXS) techniques is increasingly used to characterize the structure and interactions of biological macromolecules and their complexes in solution. It is a method of choice to characterize the flexible, partially folded and unfolded protein systems. X-ray scattering is the last resort for proteins that cannot be investigated by crystallography or NMR and acts as a complementary technique with different biophysical techniques to answer challenging scientific questions. The marriage of the X-ray scattering technique with the fourth dimension "time" yields structural dynamics and kinetics information for protein motions in hierarchical timescales from picoseconds to days. The arrival of the high-flux X-ray beam at third generation synchrotron sources, exceptional X-ray optics, state-of-the-art detectors, upgradation of X-ray scattering beamlines with microfluidics devices and advanced X-ray scattering data analysis procedures are the important reasons behind the shining years of X-ray scattering technique. The best days of the X-ray scattering technique are on the horizon with the advent of the nanofocus X-ray scattering beamlines and fourth generation X-ray lightsources, i.e., free electron lasers (XFELs). Complementary to the photon-triggered time-resolved X-ray scattering techniques, we will present an overview of the time-resolved and in-situ X-ray scattering techniques for structural dynamics of ubiquitous non-photoactive proteins.

  3. Space station application of CCD image sensors for x-ray imaging

    International Nuclear Information System (INIS)

    Charge Coupled Device (CCD) type solid state image sensors are employed in a number of space based imaging experiments and will be the basis for a camera system to acquire x-ray diffraction images on board the Space Station. This paper will present the system engineering considerations that led to the selection of CCDs over other x-ray imaging technologies and the design of the camera system. This will include discussion of the special requirements imposed by the space environment and this x-ray crystallography mission. This systems engineering discussion will be followed by a summary of high spatial resolution CCDs that are candidates for this camera, what may become available in the future, and what improvements would make CCDs even more suited to such X-ray imaging applications on the ground as well as in space

  4. One pot synthesis, molecular structure and spectroscopic studies (X-ray, IR, NMR, UV-Vis) of novel 2-(4,6-dimethoxy-1,3,5-triazin-2-yl) amino acid ester derivatives.

    Science.gov (United States)

    El-Faham, Ayman; Soliman, Saied M; Osman, Sameh M; Ghabbour, Hazem A; Siddiqui, Mohammed R H; Fun, Hoong-Kun; Albericio, Fernando

    2016-04-15

    Novel series of 2-(4,6-dimethoxy,1,3,5-triazin-2-yl) amino acid ester derivatives were synthesized using simple one pot method in methanol. The products were obtained in high yields and purities as observed from their spectral data, elemental analyses, GC-MS and X-ray crystallographic analysis. The B3LYP/6-311G(d,p) calculated molecular structures are well correlated with the geometrical parameters obtained from the X-ray analyses. The spectroscopic properties such as IR vibrational modes, NMR chemical shifts and UV-Vis electronic transitions were discussed both experimentally and theoretically. The IR vibrational frequencies showed good correlations with the experimental data (R(2)=0.9961-0.9995). The electronic spectra were assigned based on the TD-DFT results. Intense electronic transition band is calculated at 198.1 nm (f=0.1389), 204.2 nm (f=0.2053), 205.0 (f=0.1704) and 205.7 (0.2971) for compounds 6a-i, respectively. The molecular orbital energy levels contributed in the longest wavelength transition band were explained. For all compounds, the experimental wavelengths showed red shifts compared to the calculations due to the solvent effect. The NMR chemical shifts were calculated using GIAO method. The NBO analyses were performed to predict the stabilization energies due to the electron delocalization processes occur in the studied systems. PMID:26845586

  5. Probing the surface microstructure of layer-by-layer self-assembly chitosan/poly(l-glutamic acid) multilayers: A grazing-incidence small-angle X-ray scattering study.

    Science.gov (United States)

    Zhao, Nie; Yang, Chunming; Wang, Yuzhu; Zhao, Binyu; Bian, Fenggang; Li, Xiuhong; Wang, Jie

    2016-01-01

    This study characterized the surface structure of layer-by-layer self-assembly chitosan/poly(L-glutamic acid) multilayers through grazing-incidence small-angle X-ray scattering (GISAXS), X-ray reflectivity (XRR), and atomic force microscopy (AFM). A weakly long-period ordered structure along the in-plane direction was firstly observed in the polyelectrolyte multilayer by the GISAXS technique. This structure can be attributed to the specific domains on the film surface. In the domain, nanodroplets that were formed by polyelectrolyte molecules were orderly arranged along the free surface of the films. This ordered structure gradually disappeared with the increasing bilayer number because of the complex merging behavior of nanodroplets into large islands. Furthermore, resonant diffuse scattering became evident in the GISAXS patterns as the number of bilayers in the polyelectrolyte multilayer was increased. Notably, the lateral cutoff length of resonant diffuse scattering for these polyelectrolyte films was comparable with the long-period value of the ordered nanodroplets in the polyelectrolyte multilayer. Therefore, the nanodroplets could be considered as a basic transmission unit for structure propagation from the inner interface to the film surface. It suggests that the surface structure with length scale larger than the size of nanodroplets was partially complicated from the interface structure near the substrate, but surface structure smaller than the cutoff length was mainly depended on the conformation of nanodroplets. PMID:26478320

  6. Cryotomography x-ray microscopy state

    Science.gov (United States)

    Le Gros, Mark; Larabell, Carolyn A.

    2010-10-26

    An x-ray microscope stage enables alignment of a sample about a rotation axis to enable three dimensional tomographic imaging of the sample using an x-ray microscope. A heat exchanger assembly provides cooled gas to a sample during x-ray microscopic imaging.

  7. Center for X-ray Optics, 1988

    International Nuclear Information System (INIS)

    This report briefly reviews the following topics: soft-x-ray imaging; reflective optics for hard x-rays; coherent XUV sources; spectroscopy with x-rays; detectors for coronary artery imaging; synchrotron-radiation optics; and support for the advanced light source

  8. Electron beam parallel X-ray generator

    Science.gov (United States)

    Payne, P.

    1967-01-01

    Broad X ray source produces a highly collimated beam of low energy X rays - a beam with 2 to 5 arc minutes of divergence at energies between 1 and 6 keV in less than 5 feet. The X ray beam is generated by electron bombardment of a target from a large area electron gun.

  9. X-Ray Exam: Neck (For Parents)

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Neck KidsHealth > For Parents > X-Ray Exam: Neck Print A A A Text Size ... español Radiografía: cuello What It Is A neck X-ray is a safe and painless test that uses ...

  10. X-ray tracing using Geant4

    International Nuclear Information System (INIS)

    We describe an extension to the Geant4 software package that allows it to be used as a general purpose X-ray tracing package. We demonstrate the use of our extension by building a model of the X-ray optics of the X-ray observatory XMM-Newton, calculating its effective area, and comparing the results with the published calibration curves.

  11. Multigrain crystallography

    DEFF Research Database (Denmark)

    Sørensen, Henning Osholm; Schmidt, Søren; Wright, Jonathan P.;

    2012-01-01

    We summarize exploratory work on multigrain crystallography. The experimental arrangement comprises a monochromatic beam, a fully illuminated sample with up to several hundred grains in transmission geometry on a rotary table and a 2D detector. Novel algorithms are presented for indexing, integra......We summarize exploratory work on multigrain crystallography. The experimental arrangement comprises a monochromatic beam, a fully illuminated sample with up to several hundred grains in transmission geometry on a rotary table and a 2D detector. Novel algorithms are presented for indexing...... of the methodology in terms of number of grains, size of unit cell and direct space resolution. First experimental results in the fields of chemistry, structural biology and time-resolved studies in photochemistry are presented. As an outlook, the concept of TotalCrystallography is introduced, defined...

  12. Protonium X-ray spectroscopy

    CERN Document Server

    Gotta, D

    1999-01-01

    The Lyman and Balmer transitions from antiprotonic hydrogen and deuterium were studied extensively at the low-energy-antiproton ring LEAR at CERN in order to determine the strong interaction effects. A first series of experiments $9 was performed with semiconductor and gaseous X-ray detectors. In the last years of LEAR operation using a Bragg crystal spectrometer, strong interaction parameters in the 2p states of antiprotonic hydrogen and deuterium were measured $9 directly. The results of the measurements support the meson-exchange models describing the medium and long range part of the nucleon-antinucleon interaction. (39 refs).

  13. X-ray tomographic apparatus

    International Nuclear Information System (INIS)

    An x-ray tomographic system consists of a radiation source such as gamma or x radiation which produces a fan-shaped beam. The fan is wide enough to encompass the patient circle. The system further includes means for rotating the radiation source about the patient for less than a full rotation, and detectors for detecting the radiation at positions that surround the patient by 1800 plus the angle of the fan beam plus the angle between adjacent fan detectors. Attenuation data from the detectors is sorted into detector fans of attenuation data, then processed. The convolved data is back-projected into an image memory and displayed on a video monitor

  14. X-ray Pulsations in the Supersoft X-ray Binary CAL 83

    OpenAIRE

    Schmidtke, P. C.; Cowley, A. P.

    2005-01-01

    X-ray data reveal that the supersoft X-ray binary CAL 83 exhibits 38.4 minute pulsations at some epochs. These X-ray variations are similar to those found in some novae and are likely to be caused by nonradial pulsations the white dwarf. This is the first detection of pulsations in a classical supersoft X-ray binary.

  15. Ionospheric effects of solar x-rays

    Science.gov (United States)

    Danskin, Donald

    2016-07-01

    The ionospheric absorption of radio waves caused by solar x-ray bursts is measured directly by Riometers from the Canada Riometer Array. The absorption is found to be proportional to the square root of the flux intensity of the X-ray burst with time delays of 18-20 seconds between the peak X-ray emission and absorption in the ionosphere. A detailed analysis showed that some X-ray flares during 2011-2014 are more effective at producing absorption than others. Solar longitude of X-ray burst for several X-class flares shows no consistent pattern of enhancement in the absorption.

  16. Comets: mechanisms of x-ray activity

    Science.gov (United States)

    Ibadov, Subhon

    2016-07-01

    Basic mechanisms of X-ray activity of comets are considered, including D-D mechanism corresponding to generation of X-rays due to production of hot short-living plasma clumps at high-velocity collisions between cometary and interplanetary dust particles as well as M-M one corresponding to production of X-rays due to recombination of multicharge ions of solar wind plasma via charge exchange process at their collisions with molecules/atoms of the cometary atmospheres. Peculiarities of the variation of the comet X-ray spectrum and X-ray luminosity with variation of its heliocentric distance are revealed.

  17. Swift Observations of X-ray supernovae

    OpenAIRE

    Li, K. L.; Pun, Chun. S. J.

    2011-01-01

    We present a result of X-ray supernovae (SNe) survey using the Swift satellite public archive. An automatic searching program was designed to search X-ray SNe among all of the Swift archival observations between November 2004 and February 2011. Using the C++ program, 24 X-ray detectable supernovae have been found in the archive and 3 of them were newly-discovered in X-rays which are SN 1986L, SN 2003lx, and SN 2007od. In addition, SN 2003lx is a Type Ia supernova which may be the second X-ray...

  18. Symbiotic stars in X-rays

    OpenAIRE

    Luna, G. J. M.; Sokoloski, J. L.; Mukai, K; Nelson, T.

    2012-01-01

    Until recently, symbiotic binary systems in which a white dwarf accretes from a red giant were thought to be mainly a soft X-ray population. Here we describe the detection with the X-ray Telescope (XRT) on the Swift satellite of nine white dwarf symbiotics that were not previously known to be X-ray sources and one that had previously been detected as a supersoft X-ray source. The nine new X-ray detections were the result of a survey of 41 symbiotic stars, and they increase the number of symbi...

  19. Protein Crystallography in Vaccine Research and Development.

    Science.gov (United States)

    Malito, Enrico; Carfi, Andrea; Bottomley, Matthew J

    2015-06-09

    The use of protein X-ray crystallography for structure-based design of small-molecule drugs is well-documented and includes several notable success stories. However, it is less well-known that structural biology has emerged as a major tool for the design of novel vaccine antigens. Here, we review the important contributions that protein crystallography has made so far to vaccine research and development. We discuss several examples of the crystallographic characterization of vaccine antigen structures, alone or in complexes with ligands or receptors. We cover the critical role of high-resolution epitope mapping by reviewing structures of complexes between antigens and their cognate neutralizing, or protective, antibody fragments. Most importantly, we provide recent examples where structural insights obtained via protein crystallography have been used to design novel optimized vaccine antigens. This review aims to illustrate the value of protein crystallography in the emerging discipline of structural vaccinology and its impact on the rational design of vaccines.

  20. Insights into regioselective metabolism of mefenamic acid by cytochrome P450 BM3 mutants through crystallography, docking, molecular dynamics, and free energy calculations

    DEFF Research Database (Denmark)

    Capoferri, Luigi; Leth, Rasmus; Ter Haar, Ernst;

    2016-01-01

    active-site mutations such as V87I were reported to invert regioselectivity in NSAID hydroxylation. In this work, we combine crystallography and molecular simulation to study the effect of single mutations on binding and regioselective metabolism of mefenamic acid by M11 mutants. The heme domain...

  1. AXSIS: Exploring the frontiers in attosecond X-ray science, imaging and spectroscopy

    Science.gov (United States)

    Kärtner, F. X.; Ahr, F.; Calendron, A.-L.; Çankaya, H.; Carbajo, S.; Chang, G.; Cirmi, G.; Dörner, K.; Dorda, U.; Fallahi, A.; Hartin, A.; Hemmer, M.; Hobbs, R.; Hua, Y.; Huang, W. R.; Letrun, R.; Matlis, N.; Mazalova, V.; Mücke, O. D.; Nanni, E.; Putnam, W.; Ravi, K.; Reichert, F.; Sarrou, I.; Wu, X.; Yahaghi, A.; Ye, H.; Zapata, L.; Zhang, D.; Zhou, C.; Miller, R. J. D.; Berggren, K. K.; Graafsma, H.; Meents, A.; Assmann, R. W.; Chapman, H. N.; Fromme, P.

    2016-09-01

    X-ray crystallography is one of the main methods to determine atomic-resolution 3D images of the whole spectrum of molecules ranging from small inorganic clusters to large protein complexes consisting of hundred-thousands of atoms that constitute the macromolecular machinery of life. Life is not static, and unravelling the structure and dynamics of the most important reactions in chemistry and biology is essential to uncover their mechanism. Many of these reactions, including photosynthesis which drives our biosphere, are light induced and occur on ultrafast timescales. These have been studied with high time resolution primarily by optical spectroscopy, enabled by ultrafast laser technology, but they reduce the vast complexity of the process to a few reaction coordinates. In the AXSIS project at CFEL in Hamburg, funded by the European Research Council, we develop the new method of attosecond serial X-ray crystallography and spectroscopy, to give a full description of ultrafast processes atomically resolved in real space and on the electronic energy landscape, from co-measurement of X-ray and optical spectra, and X-ray diffraction. This technique will revolutionize our understanding of structure and function at the atomic and molecular level and thereby unravel fundamental processes in chemistry and biology like energy conversion processes. For that purpose, we develop a compact, fully coherent, THz-driven attosecond X-ray source based on coherent inverse Compton scattering off a free-electron crystal, to outrun radiation damage effects due to the necessary high X-ray irradiance required to acquire diffraction signals. This highly synergistic project starts from a completely clean slate rather than conforming to the specifications of a large free-electron laser (FEL) user facility, to optimize the entire instrumentation towards fundamental measurements of the mechanism of light absorption and excitation energy transfer. A multidisciplinary team formed by laser

  2. Full-field transmission x-ray imaging with confocal polycapillary x-ray optics

    OpenAIRE

    Sun, Tianxi; MacDonald, C. A.

    2013-01-01

    A transmission x-ray imaging setup based on a confocal combination of a polycapillary focusing x-ray optic followed by a polycapillary collimating x-ray optic was designed and demonstrated to have good resolution, better than the unmagnified pixel size and unlimited by the x-ray tube spot size. This imaging setup has potential application in x-ray imaging for small samples, for example, for histology specimens.

  3. Visualization of membrane protein crystals in lipid cubic phase using X-ray imaging

    International Nuclear Information System (INIS)

    A comparison of X-ray diffraction and radiographic techniques for the location and characterization of protein crystals is demonstrated on membrane protein crystals mounted within lipid cubic phase material. The focus in macromolecular crystallography is moving towards even more challenging target proteins that often crystallize on much smaller scales and are frequently mounted in opaque or highly refractive materials. It is therefore essential that X-ray beamline technology develops in parallel to accommodate such difficult samples. In this paper, the use of X-ray microradiography and microtomography is reported as a tool for crystal visualization, location and characterization on the macromolecular crystallography beamlines at the Diamond Light Source. The technique is particularly useful for microcrystals and for crystals mounted in opaque materials such as lipid cubic phase. X-ray diffraction raster scanning can be used in combination with radiography to allow informed decision-making at the beamline prior to diffraction data collection. It is demonstrated that the X-ray dose required for a full tomography measurement is similar to that for a diffraction grid-scan, but for sample location and shape estimation alone just a few radiographic projections may be required

  4. Insights into the mechanism of X-ray-induced disulfide-bond cleavage in lysozyme crystals based on EPR, optical absorption and X-ray diffraction studies

    International Nuclear Information System (INIS)

    Electron paramagnetic resonance (EPR) and online UV–visible absorption microspectrophotometry with X-ray crystallography have been used in a complementary manner to follow X-ray-induced disulfide-bond cleavage, to confirm a multi-track radiation-damage process and to develop a model of that process. Electron paramagnetic resonance (EPR) and online UV–visible absorption microspectrophotometry with X-ray crystallography have been used in a complementary manner to follow X-ray-induced disulfide-bond cleavage. Online UV–visible spectroscopy showed that upon X-irradiation, disulfide radicalization appeared to saturate at an absorbed dose of approximately 0.5–0.8 MGy, in contrast to the saturating dose of ∼0.2 MGy observed using EPR at much lower dose rates. The observations suggest that a multi-track model involving product formation owing to the interaction of two separate tracks is a valid model for radiation damage in protein crystals. The saturation levels are remarkably consistent given the widely different experimental parameters and the range of total absorbed doses studied. The results indicate that even at the lowest doses used for structural investigations disulfide bonds are already radicalized. Multi-track considerations offer the first step in a comprehensive model of radiation damage that could potentially lead to a combined computational and experimental approach to identifying when damage is likely to be present, to quantitate it and to provide the ability to recover the native unperturbed structure

  5. Future directions of electron crystallography.

    Science.gov (United States)

    Fujiyoshi, Yoshinori

    2013-01-01

    In biological science, there are still many interesting and fundamental yet difficult questions, such as those in neuroscience, remaining to be answered. Structural and functional studies of membrane proteins, which are key molecules of signal transduction in neural and other cells, are essential for understanding the molecular mechanisms of many fundamental biological processes. Technological and instrumental advancements of electron microscopy have facilitated comprehension of structural studies of biological components, such as membrane proteins. While X-ray crystallography has been the main method of structure analysis of proteins including membrane proteins, electron crystallography is now an established technique to analyze structures of membrane proteins in the lipid bilayer, which is close to their natural biological environment. By utilizing cryo-electron microscopes with helium-cooled specimen stages, structures of membrane proteins were analyzed at a resolution better than 3 Å. Such high-resolution structural analysis of membrane proteins by electron crystallography opens up the new research field of structural physiology. Considering the fact that the structures of integral membrane proteins in their native membrane environment without artifacts from crystal contacts are critical in understanding their physiological functions, electron crystallography will continue to be an important technology for structural analysis. In this chapter, I will present several examples to highlight important advantages and to suggest future directions of this technique.

  6. Nano structured materials studied by coherent X-ray diffraction

    International Nuclear Information System (INIS)

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  7. Nano structured materials studied by coherent X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gulden, Johannes

    2013-03-15

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  8. X-Ray Attenuation Cell

    Energy Technology Data Exchange (ETDEWEB)

    Ryutov, D.; Toor, A.

    2000-03-03

    To minimize the pulse-to-pulse variation, the LCLS FEL must operate at saturation, i.e. 10 orders of magnitude brighter spectral brilliance than 3rd-generation light sources. At this intensity, ultra-high vacuums and windowless transport are required. Many of the experiments, however, will need to be conducted at a much lower intensity thereby requiring a reliable means to reduce the x-ray intensity by many orders of magnitude without increasing the pulse-to-pulse variation. In this report we consider a possible solution for controlled attenuation of the LCLS x-ray radiation. We suggest using for this purpose a windowless gas-filled cell with the differential pumping. Although this scheme is easily realizable in principle, it has to be demonstrated that the attenuator can be made short enough to be practical and that the gas loads delivered to the vacuum line of sight (LOS) are acceptable. We are not going to present a final, optimized design. Instead, we will provide a preliminary analysis showing that the whole concept is robust and is worth further study. The spatial structure of the LCLS x-ray pulse at the location of the attenuator is shown in Fig. 1. The central high-intensity component, due to the FEL, has a FWHM of {approx}100 {micro}m. A second component, due to the undulator's broad band spontaneous radiation is seen as a much lower intensity ''halo'' with a FWHM of 1 mm. We discuss two versions of the attenuation cell. The first is directed towards a controlled attenuation of the FEL up to the 4 orders of magnitude in the intensity, with the spontaneous radiation halo being eliminated by collimators. In the second version, the spontaneous radiation is not sacrificed but the FEL component (as well as the first harmonic of the spontaneous radiation) gets attenuated by a more modest factor up to 100. We will make all the estimates assuming that the gas used in the attenuator is Xenon and that the energy of the FEL is 8.25 keV. At

  9. Crystallography: past and present

    Science.gov (United States)

    Hodeau, J.-L.; Guinebretiere, R.

    2007-12-01

    In the 19th century, crystallography referred to the study of crystal shapes. Such studies by Haüy and Bravais allowed the establishment of important hypotheses such as (i) “les molécules intégrantes qui sont censées être les plus petits solides que l’on puisse extraire d’un minéral” [1], (ii) the definition of the crystal lattice and (iii) “le cristal est clivable parallèlement à deux ou trois formes cristallines” [2]. This morphological crystallography defined a crystal like “a chemically homogeneous solid, wholly or partly bounded by natural planes that intersect at predetermined angles” [3]. It described the main symmetry elements and operations, nomenclatures of different crystal forms and also the theory of twinning. A breakthrough appeared in 1912 with the use of X-rays by M. von Laue and W.H. and W.L. Bragg. This experimental development allowed the determination of the atomic content of each unit cell constituting the crystal and defined a crystal as “any solid in which an atomic pattern is repeated periodically in three dimensions, that is, any solid that “diffracts” an incident X-ray beam” [3]. Mathematical tools like the Patterson methods, the direct methods, were developed. The way for solving crystalline structure was opened first for simple compounds and at that time crystallography was associated mainly with perfect crystals. In the fifties, crystallographers already had most apparatus and fundamental methods at their disposal; however, we had to wait for the development of computers to see the full use of these tools. Furthermore the development of new sources of neutrons, electrons and synchrotron X-rays allowed the studies of complex compounds like large macromolecules in biology. Nowadays, one of the new frontiers for crystallographers is to relate the crystal structure to its physical-chemical-biological properties, this means that an accurate structural determination is needed to focus on a selective part of the

  10. X-ray intensifying screens

    International Nuclear Information System (INIS)

    An x-ray intensifying screen comprises a support which has a luminescent composition comprising an isotropic phosphor and a polymer having an index of refraction within 0.02 of that of the phosphor over at least 80 percent of its emission spectrum. The support has an index of refraction up to or equal to 0.05 units higher than that of the phosphor and has a reflection optical density of at least 1.7 to light emitted by the phosphor. A preferred luminescent composition comprises Kl:Tl, Rbl:Tl at BaSrFCl:Eu mixed with two monomers such as 1-naphthylmethylmethacrylate, S(1-naphthylmethyl) thioacrylate, 1-bromo-2-naphthylacrylate, and benzyl methacrylate, coated on black anodised Al and polymerised in situ. The ratio of monomers is adjusted to give the desired refractive index. Other phosphors, polymers and supports are specified together with the preparation of the monomers and polymers. (author)

  11. X-ray flat panel detectors and X-ray tubes contributing to development of X-ray diagnostic systems

    International Nuclear Information System (INIS)

    X-ray flat panel detectors (FPDs) and X-ray tubes are key devices allowing X-ray diagnostic systems to support more sophisticated medical care. FPDs provide valuable information for the diagnosis of various diseases through the conversion of X-ray images of the human body into electronic signals, while X-ray tubes are used in a wide range of applications such as computed tomography (CT), angiography, fluoroscopy, mammography, and dental systems. Toshiba Electron Tubes and Devices Co., Ltd. has developed and commercialized FPDs providing high-quality diagnostic X-ray images with low dose exposure through the development of cutting-edge technologies including a fine crystal formation technology for cesium iodide (CsI) scintillators, thin-film transistor (TFT) arrays with photodiodes, and so on. In the field of X-ray tubes that can generate a high output of X-rays, we have developed a liquid metal hydrodynamic bearing (LM bearing) technology for various diagnostic systems including medical CT systems with a long lifetime and high rotation speed, and cardiovascular imaging systems with quiet operation. Furthermore, LM bearing technology reduces the burden on the environment by replacing insulating oil with water coolant for the cooling system and making the X-ray tubes more compact. (author)

  12. X-ray crystal structure and activity of fluorenyl-based compounds as transthyretin fibrillogenesis inhibitors.

    Science.gov (United States)

    Ciccone, Lidia; Nencetti, Susanna; Rossello, Armando; Tepshi, Livia; Stura, Enrico A; Orlandini, Elisabetta

    2016-10-01

    Transthyretin (TTR) is a 54 kDa homotetrameric protein that transports thyroxine (T4) and retinol (vitamin A), through its association with retinol binding protein (RBP). Under unknown conditions, it aggregates to form fibrils associated with TTR amyloidosis. Ligands able to inhibit fibril formation have been studied by X-ray crystallography. The use of polyethylene glycol (PEG) instead of ammonium sulphate or citrate has been evaluated as an alternative to obtain new TTR complexes with (R)-3-(9-fluoren-9-ylideneaminooxy)-2-methyl-N-(methylsulfonyl) propionamide (48R(1)) and 2-(9H-fluoren-9-ylideneaminooxy) acetic acid (ES8(2)). The previously described fluorenyl based inhibitors (S)-3-((9H-fluoren-9-ylideneamino)oxy)-2-methylpropanoic acid (6BD) and 3-((9H-fluoren-9-ylideneamino)oxy)propanoic acid (7BD) have been re-evaluated with the changed crystallization method. The new TTR complexes with compounds of the same family show that the 9-fluorenyl motif can occupy alternative hydrophobic binding sites. This augments the potential use of this scaffold to yield a large variety of differently substituted mono-aryl compounds able to inhibit TTR fibril formation. PMID:26235916

  13. Soft x-ray interferometry

    International Nuclear Information System (INIS)

    The purpose of the soft x-ray interferometry workshop held at Lawrence Berkeley Laboratory was to discuss with the scientific community the proposed technical design of the soft x-ray Fourier-transform spectrometer being developed at the ALS. Different design strategies for the instrument's components were discussed, as well as detection methods, signal processing issues, and how to meet the manufacturing tolerances that are necessary for the instrument to achieve the desired levels of performance. Workshop participants were encouraged to report on their experiences in the field of Fourier transform spectroscopy. The ALS is developing a Fourier transform spectrometer that is intended to operate up to 100 eV. The motivation is solely improved resolution and not the throughput (Jaquinot) or multiplex (Fellgett) advantage, neither of which apply for the sources and detectors used in this spectral range. The proposed implementation of this is via a Mach-Zehnder geometry that has been (1) distorted from a square to a rhombus to get grazing incidence of a suitable angle for 100 eV and (2) provided with a mirror-motion system to make the path difference between the interfering beams tunable. The experiment consists of measuring the emergent light intensity (I(x)) as a function of the path difference (x). The resolving power of the system is limited by the amount of path difference obtainable that is 1 cm (one million half-waves at 200 angstrom wavelength) in the design thus allowing a resolving power of one million. The free spectral range of the system is limited by the closeness with which the function I(x) is sampled. It is proposed to illuminate a helium absorption cell with roughly 1%-band-width light from a monochromator thus allowing one hundred aliases without spectral overlap even for sampling of I(x) at one hundredth of the Nyquist frequency

  14. Soft x-ray polarimeter laboratory tests

    Science.gov (United States)

    Murphy, Kendrah D.; Marshall, Herman L.; Schulz, Norbert S.; Jenks, Kevin; Sommer, Sophie J. B.; Marshall, Eric A.

    2010-07-01

    Multilayer-coated optics can strongly polarize X-rays and are central to a new design of a broad-band, soft X-ray polarimeter. We have begun laboratory work to verify the performance of components that could be used in future soft X-ray polarimetric instrumentation. We have reconfigured a 17 meter beamline facility, originally developed for testing transmission gratings for Chandra, to include a polarized X-ray source, an X-ray-dispersing transmission grating, and a multilayer-coated optic that illuminates a CCD detector. The X-rays produced from a Manson Model 5, multi-anode source are polarized by a multilayer-coated flat mirror. The current configuration allows for a 180 degree rotation of the source in order to rotate the direction of polarization. We will present progress in source characterization and system modulation measurements as well as null and robustness tests.

  15. X-rays for medical use

    Science.gov (United States)

    Hessenbruch, A.

    1995-11-01

    1995 is the centenary of the discovery of X-rays by the German physicist Wilhelm C Rontgen. In the past hundred years, the new rays have developed from being unknown to finding application in many walks of life, not least in medicine. This is so much so that in common speech the word `x-ray` refers not to a form of radiation but to an X-ray photograph taken for the purposes of diagnosis (as in: `I had an X-ray done to see if my leg was broken`). X-rays are now used routinely, and they are used both for diagnosis and for therapy. This paper will give an outline of the use of X-rays in medicine throughout our present century.

  16. Handbook of X-Ray Data

    CERN Document Server

    Zschornack, Günter

    2007-01-01

    This sourcebook is intended as an X-ray data reference for scientists and engineers working in the field of energy or wavelength dispersive X-ray spectrometry and related fields of basic and applied research, technology, or process and quality controlling. In a concise and informative manner, the most important data connected with the emission of characteristic X-ray lines are tabulated for all elements up to Z = 95 (Americium). This includes X-ray energies, emission rates and widths as well as level characteristics such as binding energies, fluorescence yields, level widths and absorption edges. The tabulated data are characterized and, in most cases, evaluated. Furthermore, all important processes and phenomena connected with the production, emission and detection of characteristic X-rays are discussed. This reference book addresses all researchers and practitioners working with X-ray radiation and fills a gap in the available literature.

  17. Radiation damage to nucleoprotein complexes in macromolecular crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Bury, Charles; Garman, Elspeth F.; Ginn, Helen Mary [University of Oxford, South Parks Road, Oxford OX1 3QU (United Kingdom); Ravelli, Raimond B. G. [Maastricht University, PO Box 616, Maastricht 6200 MD (Netherlands); Carmichael, Ian [University of Notre Dame, Notre Dame, IN 46556 (United States); Kneale, Geoff; McGeehan, John E., E-mail: john.mcgeehan@port.ac.uk [University of Portsmouth, King Henry 1st Street, Portsmouth PO1 2DY (United Kingdom)

    2015-01-30

    Quantitative X-ray induced radiation damage studies employing a model protein–DNA complex revealed a striking partition of damage sites. The DNA component was observed to be far more resistant to specific damage compared with the protein. Significant progress has been made in macromolecular crystallography over recent years in both the understanding and mitigation of X-ray induced radiation damage when collecting diffraction data from crystalline proteins. In contrast, despite the large field that is productively engaged in the study of radiation chemistry of nucleic acids, particularly of DNA, there are currently very few X-ray crystallographic studies on radiation damage mechanisms in nucleic acids. Quantitative comparison of damage to protein and DNA crystals separately is challenging, but many of the issues are circumvented by studying pre-formed biological nucleoprotein complexes where direct comparison of each component can be made under the same controlled conditions. Here a model protein–DNA complex C.Esp1396I is employed to investigate specific damage mechanisms for protein and DNA in a biologically relevant complex over a large dose range (2.07–44.63 MGy). In order to allow a quantitative analysis of radiation damage sites from a complex series of macromolecular diffraction data, a computational method has been developed that is generally applicable to the field. Typical specific damage was observed for both the protein on particular amino acids and for the DNA on, for example, the cleavage of base-sugar N{sub 1}—C and sugar-phosphate C—O bonds. Strikingly the DNA component was determined to be far more resistant to specific damage than the protein for the investigated dose range. At low doses the protein was observed to be susceptible to radiation damage while the DNA was far more resistant, damage only being observed at significantly higher doses.

  18. X-ray microlaminography with polycapillary optics

    Energy Technology Data Exchange (ETDEWEB)

    Dabrowski, K. M.; Dul, D. T.; Wrobel, A.; Korecki, P. [Institute of Physics, Jagiellonian University, Reymonta 4, 30-059 Krakow (Poland)

    2013-06-03

    We demonstrate layer-by-layer x-ray microimaging using polycapillary optics. The depth resolution is achieved without sample or source rotation and in a way similar to classical tomography or laminography. The method takes advantage from large angular apertures of polycapillary optics and from their specific microstructure, which is treated as a coded aperture. The imaging geometry is compatible with polychromatic x-ray sources and with scanning and confocal x-ray fluorescence setups.

  19. X-ray data booklet. Revision

    Energy Technology Data Exchange (ETDEWEB)

    Vaughan, D. (ed.)

    1986-04-01

    A compilation of data is presented. Included are properties of the elements, electron binding energies, characteristic x-ray energies, fluorescence yields for K and L shells, Auger energies, energy levels for hydrogen-, helium-, and neonlike ions, scattering factors and mass absorption coefficients, and transmission bands of selected filters. Also included are selected reprints on scattering processes, x-ray sources, optics, x-ray detectors, and synchrotron radiation facilities. (WRF)

  20. Applications of soft x-ray lasers

    Energy Technology Data Exchange (ETDEWEB)

    Skinner, C.H.

    1993-08-01

    The high brightness and short pulse duration of soft x-ray lasers provide unique advantages for novel applications. Imaging of biological specimens using x-ray lasers has been demonstrated by several groups. Other applications to fields such as chemistry, material science, plasma diagnostics, and lithography are beginning to emerge. We review the current status of soft x-ray lasers from the perspective of applications, and present an overview of the applications currently being developed.

  1. X-ray spot film device

    International Nuclear Information System (INIS)

    Improvements are described in an X-ray spot film device which is used in conjunction with an X-ray table to make a selected number of radiographic exposures on a single film and to perform fluoroscopic examinations. To date, the spot film devices consist of two X-ray field defining masks, one of which is moved manually. The present device is more convenient to use and speeds up the procedure. (U.K.)

  2. X-ray data booklet. Revision

    International Nuclear Information System (INIS)

    A compilation of data is presented. Included are properties of the elements, electron binding energies, characteristic x-ray energies, fluorescence yields for K and L shells, Auger energies, energy levels for hydrogen-, helium-, and neonlike ions, scattering factors and mass absorption coefficients, and transmission bands of selected filters. Also included are selected reprints on scattering processes, x-ray sources, optics, x-ray detectors, and synchrotron radiation facilities

  3. Topological X-Rays and MRIs

    Science.gov (United States)

    Lynch, Mark

    2002-01-01

    Let K be a compact subset of the interior of the unit disk D in the plane and suppose one can't see through the boundary of D and identify K. However, assume that one can take "topological X-rays" of D which measure the "density" of K along the lines of the X-rays. By taking these X-rays from all directions, a "topological MRI" is generated for…

  4. Synchrotron X-ray induced solution precipitation of nanoparticles

    CERN Document Server

    Lee, H J; Hwu, Y; Tsai, W L

    2003-01-01

    By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100-300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (e sub a sub q sup -), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

  5. Observation of femtosecond X-ray interactions with matter using an X-ray-X-ray pump-probe scheme.

    Science.gov (United States)

    Inoue, Ichiro; Inubushi, Yuichi; Sato, Takahiro; Tono, Kensuke; Katayama, Tetsuo; Kameshima, Takashi; Ogawa, Kanade; Togashi, Tadashi; Owada, Shigeki; Amemiya, Yoshiyuki; Tanaka, Takashi; Hara, Toru; Yabashi, Makina

    2016-02-01

    Resolution in the X-ray structure determination of noncrystalline samples has been limited to several tens of nanometers, because deep X-ray irradiation required for enhanced resolution causes radiation damage to samples. However, theoretical studies predict that the femtosecond (fs) durations of X-ray free-electron laser (XFEL) pulses make it possible to record scattering signals before the initiation of X-ray damage processes; thus, an ultraintense X-ray beam can be used beyond the conventional limit of radiation dose. Here, we verify this scenario by directly observing femtosecond X-ray damage processes in diamond irradiated with extraordinarily intense (∼10(19) W/cm(2)) XFEL pulses. An X-ray pump-probe diffraction scheme was developed in this study; tightly focused double-5-fs XFEL pulses with time separations ranging from sub-fs to 80 fs were used to excite (i.e., pump) the diamond and characterize (i.e., probe) the temporal changes of the crystalline structures through Bragg reflection. It was found that the pump and probe diffraction intensities remain almost constant for shorter time separations of the double pulse, whereas the probe diffraction intensities decreased after 20 fs following pump pulse irradiation due to the X-ray-induced atomic displacement. This result indicates that sub-10-fs XFEL pulses enable conductions of damageless structural determinations and supports the validity of the theoretical predictions of ultraintense X-ray-matter interactions. The X-ray pump-probe scheme demonstrated here would be effective for understanding ultraintense X-ray-matter interactions, which will greatly stimulate advanced XFEL applications, such as atomic structure determination of a single molecule and generation of exotic matters with high energy densities.

  6. Advanced X-ray diffractive optics

    OpenAIRE

    Vila-Comamala, J.; Jefimovs, K.; Pilvi, T.; Ritala, M; Sarkar, S S; Solak, H H; Guzenko, V.A.; Stampanoni, M.; Marone, F.; J. Raabe; G. Tzvetkov; Fink, R H; Grolimund, D.; Borca, C.N.; Kaulich, B

    2009-01-01

    X-ray microscopy greatly bene�ts from the advances in x-ray optics. At the Paul Scherrer Institut, developments in x-ray di�ractive optics include the manufacture and optimization of Fresnel zone plates (FZPs) and di�ractive optical elements for both soft and hard x-ray regimes. In particular, we demonstrate here a novel method for the production of ultra-high resolution FZPs. This technique is based on the deposition of a zone plate material (iridium) onto the sidewalls of a p...

  7. Symbiotic Stars in X-rays

    Science.gov (United States)

    Luna, G. J. M.; Sokoloski, J. L.; Mukai, K.; Nelson, T.

    2014-01-01

    Until recently, symbiotic binary systems in which a white dwarf accretes from a red giant were thought to be mainly a soft X-ray population. Here we describe the detection with the X-ray Telescope (XRT) on the Swift satellite of 9 white dwarf symbiotics that were not previously known to be X-ray sources and one that was previously detected as a supersoft X-ray source. The 9 new X-ray detections were the result of a survey of 41 symbiotic stars, and they increase the number of symbiotic stars known to be X-ray sources by approximately 30%. Swift/XRT detected all of the new X-ray sources at energies greater than 2 keV. Their X-ray spectra are consistent with thermal emission and fall naturally into three distinct groups. The first group contains those sources with a single, highly absorbed hard component, which we identify as probably coming from an accretion-disk boundary layer. The second group is composed of those sources with a single, soft X-ray spectral component, which likely arises in a region where low-velocity shocks produce X-ray emission, i.e. a colliding-wind region. The third group consists of those sources with both hard and soft X-ray spectral components. We also find that unlike in the optical, where rapid, stochastic brightness variations from the accretion disk typically are not seen, detectable UV flickering is a common property of symbiotic stars. Supporting our physical interpretation of the two X-ray spectral components, simultaneous Swift UV photometry shows that symbiotic stars with harder X-ray emission tend to have stronger UV flickering, which is usually associated with accretion through a disk. To place these new observations in the context of previous work on X-ray emission from symbiotic stars, we modified and extended the alpha/beta/gamma classification scheme for symbiotic-star X-ray spectra that was introduced by Muerset et al. based upon observations with the ROSAT satellite, to include a new sigma classification for sources with

  8. The Lunar X-ray Observatory (LXO)

    Science.gov (United States)

    Porter, F. Scott

    2008-01-01

    X-ray emission from charge exchange recombination between the highly ionized solar wind and neutral material i n Earth's magnetosheath has complicated x-ray observations of celestial objects with x-ray observatories including ROSAT, Chandra, XMM-Newton, and Suzaku. However, the charge-exchange emission can also be used as an important diagnostic of the solar-wind interacting with the magnetosheath. Soft x-ray observations from low-earth orbit or even the highly eccentric orbits of Chandra and XMM-Newton are likely superpositions of the celestial object of interest, the true extra-solar soft x-ray background, geospheric charge exchange, and heliospheric charge exchange. We show that with a small x-ray telescope placed either on the moon, in a similar vein as the Apollo ALSOP instruments, or at a stable orbit near L1, we can begin t o disentangle the complicated emission structure in the soft x-ray band. Here we present initial results of a feasibility study recently funded by NASA t o place a small x-ray telescope on the lunar surface. The telescope operates during lunar night to observe charge exchange interactions between the solar wind and magnetospheric neutrals, between the solar wind and the lunar atmosphere, and an unobstructed view of the soft x-ray background without the geospheric component.

  9. Ultrashort X-ray pulse science

    International Nuclear Information System (INIS)

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90o Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ∼ 300 fs, 30 keV (0.4 (angstrom)) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been

  10. X-ray pulsar rush in 1998

    Energy Technology Data Exchange (ETDEWEB)

    Imanishi, K.; Tsujimoto, K.; Nishiuchi, Mamiko; Yokogawa, J.; Koyama, K. [Kyoto Univ., Faculty of Science, Kyoto (Japan)

    1999-08-01

    We present recent remarkable topics about discoveries of X-ray pulsars. 1. Pulsations from two Soft Gamma-ray Repeaters: These pulsars have enormously strong magnetic field (B {approx} 10{sup 15} G), thus these are called as 'magnetar', new type of X-ray pulsars. 2. New Crab-like pulsars: These discoveries lead to suggesting universality of Crab-like pulsars. 3. An X-ray bursting millisecond pulsar: This is strong evidence for the recycle theory of generating radio millisecond pulsars. 4. X-ray pulsar rush in the SMC: This indicates the younger star formation history in the SMC. (author)

  11. Ultrashort X-ray pulse science

    Energy Technology Data Exchange (ETDEWEB)

    Chin, Alan Hap [Univ. of California, Berkeley, CA (US). Dept. of Physics; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    1998-05-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90{sup o} Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated {approx} 300 fs, 30 keV (0.4 {angstrom}) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has

  12. Imaging with x-ray lasers

    Energy Technology Data Exchange (ETDEWEB)

    Da Silva, L.B.; Cauble, B.; Frieders, G.; Koch, J.A.; MacGowan, B.J.; Matthews, D.L.; Mrowka, S.; Ress, D.; Trebes, J.E.; Weiland, T.L.

    1993-11-01

    Collisionally pumped soft x-ray lasers now operate over a wavelength range extending from 35--300 {Angstrom}. These sources have high peak brightness and are now being utilized for x-ray imaging and plasma interferometry. In this paper we will describe our efforts to probe long scalelength plasmas using Moire deflectrometry and soft x-ray imaging. The progress in the development of short pulse x-ray lasers using a double pulse irradiation technique which incorporates a travelling wave pump will also be presented.

  13. X-ray Emission from Elliptical Galaxies

    OpenAIRE

    Sarazin, Craig L.

    1996-01-01

    Elliptical galaxies are generally luminous sources of X-ray radiation, and contain large amounts of hot, interstellar gas. In the brighter X-ray galaxies, the inferred masses of hot gas are consistent with those expected given the present rates of stellar mass loss. The required rates of heating of the gas are also roughly consistent with those expected from the motions of gas losing stars. X-ray observations, particularly X-ray spectra, require a low rate of Type Ia supernova heating and che...

  14. X-ray Observations of Planetary Nebulae

    OpenAIRE

    Guerrero, M. A.; Chu, Y.-H.; Gruendl, R A

    2003-01-01

    Planetary nebulae (PNe) are an exciting addition to the zoo of X-ray sources. Recent Chandra and XMM-Newton observations have detected diffuse X-ray emission from shocked fast winds in PN interiors as well as bow-shocks of fast collimated outflows impinging on the nebular envelope. Point X-ray sources associated with PN central stars are also detected, with the soft X-ray (>0.5 keV) emission from instability shocks in the fast stellar wind itself or from a low-mass companion's coronal activit...

  15. X-ray pulsars: a review

    CERN Document Server

    Caballero, I

    2012-01-01

    Accreting X-ray pulsars are among the most luminous objects in the X-ray sky. In highly magnetized neutron stars (B~10^12 G), the flow of matter is dominated by the strong magnetic field. The general properties of accreting X-ray binaries are presented, focusing on the spectral characteristics of the systems. The use of cyclotron lines as a tool to directly measure a neutron star's magnetic field and to test the theory of accretion are discussed. We conclude with the current and future prospects for accreting X-ray binary studies.

  16. Hard X-ray Modulation Telescope

    Institute of Scientific and Technical Information of China (English)

    LU Fangjun

    2011-01-01

    The Hard X-ray Modulation Telescope (HXMT) will be China's first astronomical satellite. On board HXMT there are three kinds of slat-collimated telescopes, the High Energy X-ray Telescope (HE, 20-250 keV, 5000 cm^2), the Medium Energy X-ray Telescope (ME, 5-30 keV, 952 cm^2), and the Low Energy X-ray Telescope (LE, 1-15 keV, 384 cm^2).

  17. X-rays from the youngest stars

    Science.gov (United States)

    Feigelson, Eric D.

    1994-01-01

    The X-ray properties of classical and weak-lined T Tauri stars are briefly reviewed, emphasizing recent results from the ROSAT satellite and prospects for ASCA. The interpretation of the high level of T Tauri X-rays as enhanced solar-type magnetic activity is discussed and criticized. The census of X-ray emitters is significantly increasing estimates of galactic star formation efficiency, and X-ray emission may be important for self-regulation of star formation. ASCA images will detect star formation regions out to several kiloparsecs and will study the magnetically heated plasma around T Tauri stars. However, images will often suffer from crowding effects.

  18. Lipidic phase membrane protein serial femtosecond crystallography

    OpenAIRE

    Johansson, LC; Arnlund, D.; White, TA; Katona, G.; DePonte, DP; Weierstall, U.; Doak, RB; Shoeman, RL; Lomb, L; Malmerberg, E.; Davidsson, J; Nass, K.; Liang, MN; Andreasson, J.; Dell'Aquila, A.

    2012-01-01

    X-ray free electron laser (X-FEL)-based serial femtosecond crystallography is an emerging method with potential to rapidly advance the challenging field of membrane protein structural biology. Here we recorded interpretable diffraction data from micrometer-sized lipidic sponge phase crystals of the Blastochloris viridis photosynthetic reaction center delivered into an X-FEL beam using a sponge phase micro-jet.

  19. The success story of crystallography.

    Science.gov (United States)

    Schwarzenbach, Dieter

    2012-01-01

    Diffractionists usually place the birth of crystallography in 1912 with the first X-ray diffraction experiment of Friedrich, Knipping and Laue. This discovery propelled the mathematical branch of mineralogy to global importance and enabled crystal structure determination. Knowledge of the geometrical structure of matter at atomic resolution had revolutionary consequences for all branches of the natural sciences: physics, chemistry, biology, earth sciences and material science. It is scarcely possible for a single person in a single article to trace and appropriately value all of these developments. This article presents the limited, subjective view of its author and a limited selection of references. The bulk of the article covers the history of X-ray structure determination from the NaCl structure to aperiodic structures and macromolecular structures. The theoretical foundations were available by 1920. The subsequent success of crystallography was then due to the development of diffraction equipment, the theory of the solution of the phase problem, symmetry theory and computers. The many structures becoming known called for the development of crystal chemistry and of data banks. Diffuse scattering from disordered structures without and with partial long-range order allows determination of short-range order. Neutron and electron scattering and diffraction are also mentioned. PMID:22186283

  20. X-ray structure analysis of a metalloprotein with enhanced active-site resolution using in situ x-ray absorption near edge structure spectroscopy.

    Science.gov (United States)

    Arcovito, Alessandro; Benfatto, Maurizio; Cianci, Michele; Hasnain, S Samar; Nienhaus, Karin; Nienhaus, G Ulrich; Savino, Carmelinda; Strange, Richard W; Vallone, Beatrice; Della Longa, Stefano

    2007-04-10

    X-ray absorption spectroscopy is exquisitely sensitive to the coordination geometry of an absorbing atom and therefore allows bond distances and angles of the surrounding atomic cluster to be measured with atomic resolution. By contrast, the accuracy and resolution of metalloprotein active sites obtainable from x-ray crystallography are often insufficient to analyze the electronic properties of the metals that are essential for their biological functions. Here, we demonstrate that the combination of both methods on the same metalloprotein single crystal yields a structural model of the protein with exceptional active-site resolution. To this end, we have collected an x-ray diffraction data set to 1.4-A resolution and Fe K-edge polarized x-ray absorption near edge structure (XANES) spectra on the same cyanomet sperm whale myoglobin crystal. The XANES spectra were quantitatively analyzed by using a method based on the multiple scattering approach, which yielded Fe-heme structural parameters with +/-(0.02-0.07)-A accuracy on the atomic distances and +/-7 degrees on the Fe-CN angle. These XANES-derived parameters were subsequently used as restraints in the crystal structure refinement. By combining XANES and x-ray diffraction, we have obtained an cyanomet sperm whale myoglobin structural model with a higher precision of the bond lengths and angles at the active site than would have been possible with crystallographic analysis alone.

  1. X-ray imaging using a tunable coherent X-ray source based on parametric X-ray radiation

    International Nuclear Information System (INIS)

    A novel X-ray source based on parametric X-ray radiation (PXR) has been employed for X-ray imaging at the Laboratory for Electron Beam Research and Application (LEBRA), Nihon University. Notable features of PXR are tunable energy, monochromaticity with spatial chirp, narrow local bandwidth and spatial coherence. Since the X-ray beam from the PXR system has a large irradiation area with uniform flux density, the PXR-based source is suited for X-ray imaging, especially for application to phase-contrast imaging. Despite the cone-like X-ray beam, diffraction-enhanced imaging (DEI) can be employed as a phase contrast imaging technique. DEI experiments were performed using 14- to 34-keV X-rays and the phase-gradient images were obtained. The results demonstrated the capability of PXR as an X-ray source for phase-contrast imaging with a large irradiation field attributed to the cone-beam effect. Given the significant properties of the LEBRA-PXR source, the result suggests the possible construction of a compact linac-driven PXR-Imaging instrument and its application to medical diagnoses

  2. Graphene-based microfluidics for serial crystallography.

    Science.gov (United States)

    Sui, Shuo; Wang, Yuxi; Kolewe, Kristopher W; Srajer, Vukica; Henning, Robert; Schiffman, Jessica D; Dimitrakopoulos, Christos; Perry, Sarah L

    2016-08-01

    Microfluidic strategies to enable the growth and subsequent serial crystallographic analysis of micro-crystals have the potential to facilitate both structural characterization and dynamic structural studies of protein targets that have been resistant to single-crystal strategies. However, adapting microfluidic crystallization platforms for micro-crystallography requires a dramatic decrease in the overall device thickness. We report a robust strategy for the straightforward incorporation of single-layer graphene into ultra-thin microfluidic devices. This architecture allows for a total material thickness of only ∼1 μm, facilitating on-chip X-ray diffraction analysis while creating a sample environment that is stable against significant water loss over several weeks. We demonstrate excellent signal-to-noise in our X-ray diffraction measurements using a 1.5 μs polychromatic X-ray exposure, and validate our approach via on-chip structure determination using hen egg white lysozyme (HEWL) as a model system. Although this work is focused on the use of graphene for protein crystallography, we anticipate that this technology should find utility in a wide range of both X-ray and other lab on a chip applications. PMID:27241728

  3. On the universal X-ray luminosity function of binary X-ray sources in galaxies

    OpenAIRE

    Postnov, K. A.

    2002-01-01

    The empirically determined universal power-law shape of X-ray luminosity function of high mass X-ray binaries in galaxies is explained by fundamental mass-luminosity and mass-radius relations for massive stars.

  4. Discrete tomographic reconstruction of 2D polycrystal orientation maps from X-ray diffraction projections using Gibbs priors

    DEFF Research Database (Denmark)

    Rodek, L.; Knudsen, E.; Poulsen, H.F.;

    2005-01-01

    The determination of crystalline structures is a demanding and fundamental task of crystallography. This paper offers a new approach for rendering a 2D grain map of a polycrystal based on an orientation map reconstructed from X-ray diffraction patterns. The orientation map is produced by a Bayesian...

  5. SN X-ray Progenitor?

    Science.gov (United States)

    2008-01-01

    Identifying stars that explode, right before they explode, is a tricky proposition since the end of starlife comes swiftly: in thermonuclear deflagrations, in nuclear exhaustion, or maybe in a rapid swirling merger of two dead stellar cores. On the right in the image above is an image of the galaxy NGC 1404 taken by the UV/optical Telescope (UVOT) on the Swift observatory. The circle surrounds SN 2007on, a supernova of Type Ia produced by the explosion of a white dwarf star in a binary system. These types of supernovae are important since they are believed to be 'standard candles', events which have the same intrinsic brightness which can serve as an important yardstick to measure cosmic distances. On the left is an image of the same galaxy taken by the Chandra X-ray observatory four years before the supernova. Conspicuous in the SN source circle is a bright source in the Chandra image, believed to be emission from a compact object+normal star companion: a similar system to the supposed precursor of SN 2007on. If true this would be the first time a Type Ia supernova precursor has ever been seen. But astronomers are still debating whether the Chandra source really is the precursor or not; it seems there's a slight but significant difference in the location of the Chandra source and the supernova. Stay tuned for more developments.

  6. X-ray radiography facility

    International Nuclear Information System (INIS)

    The paper described a radiographic apparatus containing a radiation source, a diaphragm with collimating windows and a cassette holder with a cassette for the X-ray film. In order to increase the efficiency and quality of monitoring, the diaphragm and the cassette are made in the form of cylindrical shells, the centre of curvature of which coincides with the position of the radiation source focus. Each collimating window of the diaphragm is made in the form of two coaxially connected truncated cones, joined at the large bases in such a way that the angle at the vertex of the cone nearer the source is not less than the central angle with the vertex at the focus of the radiation source supported by the larger base, and 15-300 less than the angle at the vertex of the cone further from the source. By this means monitoring efficiency is increased by a factor of 1.5-2 and the quality of the radiographs improved. The apparatus is used for flaw detection in cylindrical objects. (author)

  7. X-ray computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Kalender, Willi A [Institute of Medical Physics, University Erlangen-Nuernberg, Henkestr. 91, D-91052 Erlangen (Germany)

    2006-07-07

    X-ray computed tomography (CT), introduced into clinical practice in 1972, was the first of the modern slice-imaging modalities. To reconstruct images mathematically from measured data and to display and to archive them in digital form was a novelty then and is commonplace today. CT has shown a steady upward trend with respect to technology, performance and clinical use independent of predictions and expert assessments which forecast in the 1980s that it would be completely replaced by magnetic resonance imaging. CT not only survived but exhibited a true renaissance due to the introduction of spiral scanning which meant the transition from slice-by-slice imaging to true volume imaging. Complemented by the introduction of array detector technology in the 1990s, CT today allows imaging of whole organs or the whole body in 5 to 20 s with sub-millimetre isotropic resolution. This review of CT will proceed in chronological order focussing on technology, image quality and clinical applications. In its final part it will also briefly allude to novel uses of CT such as dual-source CT, C-arm flat-panel-detector CT and micro-CT. At present CT possibly exhibits a higher innovation rate than ever before. In consequence the topical and most recent developments will receive the greatest attention. (review)

  8. Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

    2016-08-09

    A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

  9. Single molecule imaging with longer x-ray laser pulses

    CERN Document Server

    Martin, Andrew V; Caleman, Carl; Quiney, Harry M

    2015-01-01

    In serial femtosecond crystallography, x-ray laser pulses do not need to outrun all radiation damage processes because Bragg diffraction exceeds the damage-induced background scattering for longer pulses ($\\sim$ 50--100 fs). This is due to a "self-gating pulse" effect whereby damage terminates Bragg diffraction prior to the pulse completing its passage through the sample, as if that diffraction were produced by a shorter pulse of equal fluence. We show here that a similar gating effect applies to single molecule diffraction with respect to spatially uncorrelated damage processes like ionization and ion diffusion. The effect is clearly seen in calculations of the diffraction contrast, by calculating the diffraction of average structure separately to the diffraction from statistical fluctuations of the structure due to damage ("damage noise"). Our results suggest that sub-nanometer single molecule imaging with longer pulses, like those produced at currently operating facilities, should not yet be ruled out. The...

  10. Accelerator-driven X-ray Sources

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, Dinh Cong [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-11-09

    After an introduction which mentions x-ray tubes and storage rings and gives a brief review of special relativity, the subject is treated under the following topics and subtopics: synchrotron radiation (bending magnet radiation, wiggler radiation, undulator radiation, brightness and brilliance definition, synchrotron radiation facilities), x-ray free-electron lasers (linac-driven X-ray FEL, FEL interactions, self-amplified spontaneous emission (SASE), SASE self-seeding, fourth-generation light source facilities), and other X-ray sources (energy recovery linacs, Inverse Compton scattering, laser wakefield accelerator driven X-ray sources. In summary, accelerator-based light sources cover the entire electromagnetic spectrum. Synchrotron radiation (bending magnet, wiggler and undulator radiation) has unique properties that can be tailored to the users’ needs: bending magnet and wiggler radiation is broadband, undulator radiation has narrow spectral lines. X-ray FELs are the brightest coherent X-ray sources with high photon flux, femtosecond pulses, full transverse coherence, partial temporal coherence (SASE), and narrow spectral lines with seeding techniques. New developments in electron accelerators and radiation production can potentially lead to more compact sources of coherent X-rays.

  11. X-ray topography and multiple diffraction

    International Nuclear Information System (INIS)

    A short summary on X-ray topography, which is based on the dynamical theory of X-ray diffraction, is made. The applications and properties related to the use of the multiple diffraction technique are analized and discussed. (L.C.)

  12. Soft x rays for radiobiological studies

    International Nuclear Information System (INIS)

    Lethal effects and chromosome aberrations induced in cells exposed to low energy (soft) X rays demonstrated that these relatively low energy X rays are just as effective as those of higher energy for radiobiological studies, and even more effective for irradiating cultured mammalian cells than laboratory animals. (author)

  13. Coccidioidomycosis - chest x-ray (image)

    Science.gov (United States)

    This chest x-ray shows the affects of a fungal infection, coccidioidomycosis. In the middle of the left lung (seen on the ... defined borders. Other diseases that may explain these x-ray findings include lung abscesses, chronic pulmonary tuberculosis, chronic ...

  14. X-Ray Detection Visits the Classroom

    Science.gov (United States)

    Peralta, Luis; Farinha, Ana; Pinto, Ana

    2008-01-01

    Film has been used to detect x-rays since the early days of their discovery by Rontgen. Although nowadays superseded by other techniques, film still provides a cheap means of x-ray detection, making it attractive in high-school or undergraduate university courses. If some sort of quantitative result is required, the film's optical absorbance or…

  15. Adenocarcinoma - chest x-ray (image)

    Science.gov (United States)

    This chest x-ray shows adenocarcinoma of the lung. There is a rounded light spot in the right upper lung (left side ... density. Diseases that may cause this type of x-ray result would be tuberculous or fungal granuloma, and ...

  16. Tracing the X-Ray Trail

    Science.gov (United States)

    What you need to know about… Tracing the X-ray Trail If you’ve just completed an x-ray, computed tomography (CT), magnetic resonance (MR) Start here! or other diagnostic imaging procedure, you probably want to know when you will ... los rayos X Si acaba de hacerse una radiografía, tomografía ¡Empezar ...

  17. Proton induced X-ray emission analysis

    International Nuclear Information System (INIS)

    The developments in proton induced X-ray emission analysis are reviewed. Techniques for analyzing thick and thin samples of different origin are described. Discussions on the application of proton induced X-ray emission analysis in different fields, comparison of the sensitivity of this method with other analytical techniques, its limitations and possible improvements are presented

  18. X-ray scattering measurements from thin-foil x-ray mirrors

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; BYRNAK, BP; Hornstrup, Allan;

    1992-01-01

    Thin foil X-ray mirrors are to be used as the reflecting elements in the telescopes of the X-ray satellites Spectrum-X-Gamma (SRG) and ASTRO-D. High resolution X-ray scattering measurements from the Au coated and dip-lacquered Al foils are presented. These were obtained from SRG mirrors positione...

  19. Characterization of Metalloproteins and Biomaterials by X-ray Absorption Spectroscopy and X-ray Diffraction

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

    This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X-ray crystallo...

  20. Soft X-Ray Spectra of AGN Discovered Via Their Hard X-Ray

    Science.gov (United States)

    Schwartz, Daniel

    1998-01-01

    This final report is a study of the Active Galactic Nuclei (AGN). Investigation of the soft x-ray spectra of AGN were performed by using their hard x-ray emission. ROSAT observations of AGN was also performed, which allowed for the study of these x-ray spectra and the structures of 7 clusters of galaxies.

  1. X-ray devices contributing to sophistication of X-ray diagnostic systems

    International Nuclear Information System (INIS)

    X-ray tubes to generate X-rays, as well as X-ray image intensifiers (I.I.s) and X-ray flat panel detectors (FPDs) to convert X-ray images into electronic signals, are key devices in X-ray diagnostic systems, which are playing a major role in the advancement of diagnosis and treatment. Toshiba Electron Tubes and Devices Co., Ltd. has been offering optimal products incorporating the most advanced technologies to customers through continuous technological innovations. These include a high-sensitivity technology for X-ray I.I.s and X-ray FPDs to suppress patient exposure doses, a focal spot design technology for X-ray tubes and high-resolution technologies for X-ray I.I.s and X-ray FPDs that enhance image quality and make it possible to detect smaller lesion areas, and a noise reduction technology for X-ray tubes to realize a comfortable medical environment with reduced stress on both patients and medical staff. (author)

  2. An X-ray scanner prototype based on a novel hybrid gaseous detector

    CERN Document Server

    Iacobaeus, C; Lund-Jensen, B; Peskov, Vladimir

    2007-01-01

    We have developed a prototype of a new type of hybrid X-ray detector. It contains a thin wall (few μm) edge- illuminated lead glass capillary plate (acting as a converter of X-rays photons to primary electrons) combined with a microgap parallel-plate avalanche chamber operating in various gas mixtures at 1 atm. The operation of these converters was studied in a wide range of X-ray energies (from 6 to 60 keV) at incident angles varying from 0° to 90°. The detection efficiency, depending on the geometry, photon's energy, incident angle and the mode of operation, was between a few and 40%. The position resolution achieved was 50 μm in digital form and was practically independent of the photon's energy or gas mixture. The developed detector may open new possibilities for medical imaging, for example in mammography, portal imaging, radiography (including security devices), crystallography and many other applications.

  3. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex.

    Science.gov (United States)

    Zhou, X Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W; Suino-Powell, Kelly M; Boutet, Sébastien; Williams, Garth J; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N; Spence, John C H; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C; Cherezov, Vadim; Melcher, Karsten; Xu, H Eric

    2016-01-01

    Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes. PMID:27070998

  4. Time-resolved protein nanocrystallography using an X-ray free-electron laser

    Science.gov (United States)

    Aquila, Andrew; Hunter, Mark S.; Doak, R. Bruce; Kirian, Richard A.; Fromme, Petra; White, Thomas A.; Andreasson, Jakob; Arnlund, David; Bajt, Saša; Barends, Thomas R. M.; Barthelmess, Miriam; Bogan, Michael J.; Bostedt, Christoph; Bottin, Hervé; Bozek, John D.; Caleman, Carl; Coppola, Nicola; Davidsson, Jan; DePonte, Daniel P.; Elser, Veit; Epp, Sascha W.; Erk, Benjamin; Fleckenstein, Holger; Foucar, Lutz; Frank, Matthias; Fromme, Raimund; Graafsma, Heinz; Grotjohann, Ingo; Gumprecht, Lars; Hajdu, Janos; Hampton, Christina Y.; Hartmann, Andreas; Hartmann, Robert; Hau-Riege, Stefan; Hauser, Günter; Hirsemann, Helmut; Holl, Peter; Holton, James M.; Hömke, André; Johansson, Linda; Kimmel, Nils; Kassemeyer, Stephan; Krasniqi, Faton; Kühnel, Kai-Uwe; Liang, Mengning; Lomb, Lukas; Malmerberg, Erik; Marchesini, Stefano; Martin, Andrew V.; Maia, Filipe R.N.C.; Messerschmidt, Marc; Nass, Karol; Reich, Christian; Neutze, Richard; Rolles, Daniel; Rudek, Benedikt; Rudenko, Artem; Schlichting, Ilme; Schmidt, Carlo; Schmidt, Kevin E.; Schulz, Joachim; Seibert, M. Marvin; Shoeman, Robert L.; Sierra, Raymond; Soltau, Heike; Starodub, Dmitri; Stellato, Francesco; Stern, Stephan; Strüder, Lothar; Timneanu, Nicusor; Ullrich, Joachim; Wang, Xiaoyu; Williams, Garth J.; Weidenspointner, Georg; Weierstall, Uwe; Wunderer, Cornelia; Barty, Anton; Spence, John C. H.; Chapman, Henry N.

    2012-01-01

    We demonstrate the use of an X-ray free electron laser synchronized with an optical pump laser to obtain X-ray diffraction snapshots from the photoactivated states of large membrane protein complexes in the form of nanocrystals flowing in a liquid jet. Light-induced changes of Photosystem I-Ferredoxin co-crystals were observed at time delays of 5 to 10 µs after excitation. The result correlates with the microsecond kinetics of electron transfer from Photosystem I to ferredoxin. The undocking process that follows the electron transfer leads to large rearrangements in the crystals that will terminally lead to the disintegration of the crystals. We describe the experimental setup and obtain the first time-resolved femtosecond serial X-ray crystallography results from an irreversible photo-chemical reaction at the Linac Coherent Light Source. This technique opens the door to time-resolved structural studies of reaction dynamics in biological systems. PMID:22330507

  5. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    Science.gov (United States)

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang, Rong

    2007-01-01

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  6. Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser.

    Science.gov (United States)

    Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; Kick, Leonhard M; Gati, Cornelius; Nelson, Garrett; Deupi, Xavier; Standfuss, Jörg; Schertler, Gebhard; Panneels, Valérie

    2015-07-01

    Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.

  7. An X-ray view of quasars

    CERN Document Server

    Singh, K P

    2013-01-01

    I present an overview of observational studies of quasars of all types, with particular emphasis on X-ray observational studies. The presentation is based on the most popularly accepted unified picture of quasars - collectively referred to as AGN (active galactic nuclei) in this review. Characteristics of X-ray spectra and X-ray variability obtained from various X-ray satellites over the last 5 decades have been presented and discussed. The contribution of AGN in understanding the cosmic X-ray background is discussed very briefly. Attempt has been made to provide up-to-date information; however, this is a vast subject and this presentation is not intended to be comprehensive.

  8. X-ray Fourier ptychographic microscopy

    CERN Document Server

    Simons, H; Guigay, J P; Detlefs, C

    2016-01-01

    Following the recent developement of Fourier ptychographic microscopy (FPM) in the visible range by Zheng et al. (2013), we propose an adaptation for hard x-rays. FPM employs ptychographic reconstruction to merge a series of low-resolution, wide field of view images into a high-resolution image. In the x-ray range this opens the possibility to overcome the limited numerical aperture of existing x-ray lenses. Furthermore, digital wave front correction (DWC) may be used to charaterize and correct lens imperfections. Given the diffraction limit achievable with x-ray lenses (below 100 nm), x-ray Fourier ptychographic microscopy (XFPM) should be able to reach resolutions in the 10 nm range.

  9. High Energy Vision: Processing X-rays

    CERN Document Server

    DePasquale, Joseph; Edmonds, Peter

    2015-01-01

    Astronomy is by nature a visual science. The high quality imagery produced by the world's observatories can be a key to effectively engaging with the public and helping to inspire the next generation of scientists. Creating compelling astronomical imagery can, however, be particularly challenging in the non-optical wavelength regimes. In the case of X-ray astronomy, where the amount of light available to create an image is severely limited, it is necessary to employ sophisticated image processing algorithms to translate light beyond human vision into imagery that is aesthetically pleasing while still being scientifically accurate. This paper provides a brief overview of the history of X-ray astronomy leading to the deployment of NASA's Chandra X-ray Observatory, followed by an examination of the specific challenges posed by processing X-ray imagery. The authors then explore image processing techniques used to mitigate such processing challenges in order to create effective public imagery for X-ray astronomy. ...

  10. X-Rays from Green Pea Analogs

    Science.gov (United States)

    Brorby, Matthew

    2014-09-01

    X-rays may have contributed to the heating and reionization of the IGM in the early universe. High mass X-ray binaries (HMXB) within small, low-metallicity galaxies are expected to be the main source of X-rays at this time. Since studying these high-redshift galaxies is currently impossible, we turn to local analogs that have the same properties the galaxies in the early are expected to have. A number of recent studies have shown an enhanced number of HMXBs in nearby low metallicity galaxies. We propose to observe a sample of metal-deficient luminous compact galaxies (LCG) in order to determine if the X-ray luminosity is enhanced relative to SFR, thereby providing further evidence to the importance of X-rays in the early universe.

  11. The X-ray imager on AXO

    DEFF Research Database (Denmark)

    Budtz-Jørgensen, Carl; Kuvvetli, Irfan; Westergaard, Niels Jørgen Stenfeldt;

    2001-01-01

    DSRI has initiated a development program of CZT X-ray and gamma-ray detectors employing strip readout techniques. A dramatic improvement of the energy response was found operating the detectors as the so-called drift detectors. For the electronic readout, modern ASIC chips were investigated....... Modular design and the low-power electronics will make large area detectors using the drift strip method feasible. The performance of a prototype CZT system will be presented and discussed. One such detector system has been proposed for future space missions: the X-Ray Imager (XRI) on the Atmospheric X-ray...... Observatory (AXO), which is a mission proposed to the Danish Small Satellite Program and is dedicated to observations of X-ray generating processes in the Earth's atmosphere. Of special interest will be simultaneous optical and X-ray observations of sprites that are flashes appearing directly above an active...

  12. Resonant elastic X-ray scattering in chemistry and materials science

    Science.gov (United States)

    Helliwell, J. R.; Helliwell, M.; Kaucic, V.; Logar, N. Z.

    2012-06-01

    The applications of anomalous scattering for locating metal atoms and discriminating between different elements has increased when optimised with synchrotron X-radiation.The on-resonance effect enhances the targeted elemental signal and allows small occupancies to be determined, including in situations of a mixed metal population at a single atomic site. Thus the applications of resonant elastic X-ray scattering in biological, inorganic and materials chemistry is being widely applied to single crystals, which is our emphasis, but also powders, fibres, solutions, amorphous and thin film states of matter. Recent developments have included the use of high photon energies (upto 100 keV) as well as softer X-rays (2 keV). The various instrument and technical capabilities have improved in the last 15 years. This ease of measurement of the resonant scattering signals along with absorption edge shifts indicates an expansion to the measurement of multiple data sets, to allow monitoring of redox changes. Whilst crystal structure determination in biological crystallography has been revolutionised by the MAD method, it is not a requirement for chemical or materials crystallography, as other phasing techniques are routine. Synchrotron source upgrades will allow nano-sized X-ray beams to be more widely available. The new X-ray lasers suggest new capabilities too.

  13. From lows to highs: using low-resolution models to phase X-ray data

    International Nuclear Information System (INIS)

    An unusual example of how virus structure determination pushes the limits of the molecular replacement method is presented. The study of virus structures has contributed to methodological advances in structural biology that are generally applicable (molecular replacement and noncrystallographic symmetry are just two of the best known examples). Moreover, structural virology has been instrumental in forging the more general concept of exploiting phase information derived from multiple structural techniques. This hybridization of structural methods, primarily electron microscopy (EM) and X-ray crystallography, but also small-angle X-ray scattering (SAXS) and nuclear magnetic resonance (NMR) spectroscopy, is central to integrative structural biology. Here, the interplay of X-ray crystallography and EM is illustrated through the example of the structural determination of the marine lipid-containing bacteriophage PM2. Molecular replacement starting from an ∼13 Å cryo-EM reconstruction, followed by cycling density averaging, phase extension and solvent flattening, gave the X-ray structure of the intact virus at 7 Å resolution This in turn served as a bridge to phase, to 2.5 Å resolution, data from twinned crystals of the major coat protein (P2), ultimately yielding a quasi-atomic model of the particle, which provided significant insights into virus evolution and viral membrane biogenesis

  14. Protein crystal structure from non-oriented, single-axis sparse X-ray data

    Directory of Open Access Journals (Sweden)

    Jennifer L. Wierman

    2016-01-01

    Full Text Available X-ray free-electron lasers (XFELs have inspired the development of serial femtosecond crystallography (SFX as a method to solve the structure of proteins. SFX datasets are collected from a sequence of protein microcrystals injected across ultrashort X-ray pulses. The idea behind SFX is that diffraction from the intense, ultrashort X-ray pulses leaves the crystal before the crystal is obliterated by the effects of the X-ray pulse. The success of SFX at XFELs has catalyzed interest in analogous experiments at synchrotron-radiation (SR sources, where data are collected from many small crystals and the ultrashort pulses are replaced by exposure times that are kept short enough to avoid significant crystal damage. The diffraction signal from each short exposure is so `sparse' in recorded photons that the process of recording the crystal intensity is itself a reconstruction problem. Using the EMC algorithm, a successful reconstruction is demonstrated here in a sparsity regime where there are no Bragg peaks that conventionally would serve to determine the orientation of the crystal in each exposure. In this proof-of-principle experiment, a hen egg-white lysozyme (HEWL crystal rotating about a single axis was illuminated by an X-ray beam from an X-ray generator to simulate the diffraction patterns of microcrystals from synchrotron radiation. Millions of these sparse frames, typically containing only ∼200 photons per frame, were recorded using a fast-framing detector. It is shown that reconstruction of three-dimensional diffraction intensity is possible using the EMC algorithm, even with these extremely sparse frames and without knowledge of the rotation angle. Further, the reconstructed intensity can be phased and refined to solve the protein structure using traditional crystallographic software. This suggests that synchrotron-based serial crystallography of micrometre-sized crystals can be practical with the aid of the EMC algorithm even in cases

  15. X-ray structure determination and deuteration of nattokinase

    Energy Technology Data Exchange (ETDEWEB)

    Yanagisawa, Yasuhide [Chiba Institute of Science, 15-8 Shiomi-cho, Cho-shi, Chiba 288-025 (Japan); Chatake, Toshiyuki, E-mail: chatake@rri.kyoto-u.ac.jp [Kyoto University, Asashironishi 2, Kumatori, Osaka 590-0494 (Japan); Naito, Sawa; Ohsugi, Tadanori; Yatagai, Chieko; Sumi, Hiroyuki [Kurashiki University of Science and the Arts, 2640 Nishinoura, Tsurajima-cho, Kurashiki, Okayama 712-8505 (Japan); Kawaguchi, Akio [Kyoto University, Asashironishi 2, Kumatori, Osaka 590-0494 (Japan); Chiba-Kamosida, Kaori [Nippon Advanced Technology Co. Ltd, J-PARC, 2-4 Shirane Shirakata, Tokai, Ibaraki 319-1195 (Japan); Ogawa, Megumi; Adachi, Tatsumi [Chiba Institute of Science, 15-8 Shiomi-cho, Cho-shi, Chiba 288-025 (Japan); Morimoto, Yukio [Kyoto University, Asashironishi 2, Kumatori, Osaka 590-0494 (Japan)

    2013-11-01

    X-ray structure determination and deuteration of nattokinase were performed to facilitate neutron crystallographic analysis. Nattokinase (NK) is a strong fibrinolytic enzyme, which is produced in abundance by Bacillus subtilis natto. Although NK is a member of the subtilisin family, it displays different substrate specificity when compared with other subtilisins. The results of molecular simulations predict that hydrogen arrangements around Ser221 at the active site probably account for the substrate specificity of NK. Therefore, neutron crystallographic analysis should provide valuable information that reveals the enzymatic mechanism of NK. In this report, the X-ray structure of the non-hydrogen form of undeuterated NK was determined, and the preparation of deuterated NK was successfully achieved. The non-hydrogen NK structure was determined at 1.74 Å resolution. The three-dimensional structures of NK and subtilisin E from Bacillus subtilis DB104 are near identical. Deuteration of NK was carried out by cultivating Bacillus subtilis natto in deuterated medium. The D{sub 2}O resistant strain of Bacillus subtilis natto was obtained by successive cultivation rounds, in which the concentration of D{sub 2}O in the medium was gradually increased. NK was purified from the culture medium and its activity was confirmed by the fibrin plate method. The results lay the framework for neutron protein crystallography analysis.

  16. Evolution of Substrate Specificity within a Diverse Family of [beta/alpha]-Barrel-fold Basic Amino Acid Decarboxylases X-ray Structure Determination of Enzymes with Specificity for L-Arginine and Carboxynorspermidine

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Xiaoyi; Lee, Jeongmi; Michael, Anthony J.; Tomchick, Diana R.; Goldsmith, Elizabeth J.; Phillips, Margaret A. (Sungkyunkwan); (UTSMC)

    2010-08-26

    Pyridoxal 5{prime}-phosphate (PLP)-dependent basic amino acid decarboxylases from the {beta}/{alpha}-barrel-fold class (group IV) exist in most organisms and catalyze the decarboxylation of diverse substrates, essential for polyamine and lysine biosynthesis. Herein we describe the first x-ray structure determination of bacterial biosynthetic arginine decarboxylase (ADC) and carboxynorspermidine decarboxylase (CANSDC) to 2.3- and 2.0-{angstrom} resolution, solved as product complexes with agmatine and norspermidine. Despite low overall sequence identity, the monomeric and dimeric structures are similar to other enzymes in the family, with the active sites formed between the {beta}/{alpha}-barrel domain of one subunit and the {beta}-barrel of the other. ADC contains both a unique interdomain insertion (4-helical bundle) and a C-terminal extension (3-helical bundle) and it packs as a tetramer in the asymmetric unit with the insertions forming part of the dimer and tetramer interfaces. Analytical ultracentrifugation studies confirmed that the ADC solution structure is a tetramer. Specificity for different basic amino acids appears to arise primarily from changes in the position of, and amino acid replacements in, a helix in the {beta}-barrel domain we refer to as the 'specificity helix.' Additionally, in CANSDC a key acidic residue that interacts with the distal amino group of other substrates is replaced by Leu{sup 314}, which interacts with the aliphatic portion of norspermidine. Neither product, agmatine in ADC nor norspermidine in CANSDC, form a Schiff base to pyridoxal 5{prime}-phosphate, suggesting that the product complexes may promote product release by slowing the back reaction. These studies provide insight into the structural basis for the evolution of novel function within a common structural-fold.

  17. An experimental measurement of metal multilayer x-ray reflectivity degradation due to intense x-ray flux

    International Nuclear Information System (INIS)

    The degradation of the x-ray reflection characteristics of metal multilayer Bragg diffractors due to intense x-ray flux was investigated. The Z-pinch plasma produced by PROTO II of Sandia National Laboratories, Albuquerque, New Mexico, was used as the source. The plasma generated total x-ray yields of as much as 40 kJ with up to 15 kJ in the neon hydrogen- and helium-like resonance lines in nominal 20-ns pulses. Molybdenum-carbon, palladium-carbon, and tungsten-carbon metal multilayers were placed at 15 and 150 cm from the plasma center. The multilayers were at nominal angles of 50 and 100 to diffract the neon resonance lines. The time-integrated x-ray reflection of the metal multilayers was monitored by x-ray film. A fluorescer-fiber optic-visible streak camera detector system was then used to monitor the time-resolved x-ray reflection characteristics of 135 A- 2d tungsten-carbon multilayers. A large specular component in the reflectivity prevented determination of the rocking curve of the multilayer. For a neon implosion onto a vanadium-doped polyacrylic acid foam target shot, detailed modeling was attempted. The spectral flux was determined with data from 5 XRD channels and deconvolved using the code SHAZAM. The observed decay in reflectivity was assumed to correspond to the melting of the first tungsten layer. A ''conduction factor'' of 82 was required to manipulate the heat loading of the first tungsten layer such that the time of melting corresponded to the observed decay. The power at destruction was 141 MW/cm2 and the integrated energy at destruction was 2.0 J/cm2. 82 refs., 66 figs., 10 tabs

  18. An experimental measurement of metal multilayer x-ray reflectivity degradation due to intense x-ray flux

    Energy Technology Data Exchange (ETDEWEB)

    Hockaday, M.Y.P.

    1987-06-01

    The degradation of the x-ray reflection characteristics of metal multilayer Bragg diffractors due to intense x-ray flux was investigated. The Z-pinch plasma produced by PROTO II of Sandia National Laboratories, Albuquerque, New Mexico, was used as the source. The plasma generated total x-ray yields of as much as 40 kJ with up to 15 kJ in the neon hydrogen- and helium-like resonance lines in nominal 20-ns pulses. Molybdenum-carbon, palladium-carbon, and tungsten-carbon metal multilayers were placed at 15 and 150 cm from the plasma center. The multilayers were at nominal angles of 5/sup 0/ and 10/sup 0/ to diffract the neon resonance lines. The time-integrated x-ray reflection of the metal multilayers was monitored by x-ray film. A fluorescer-fiber optic-visible streak camera detector system was then used to monitor the time-resolved x-ray reflection characteristics of 135 A- 2d tungsten-carbon multilayers. A large specular component in the reflectivity prevented determination of the rocking curve of the multilayer. For a neon implosion onto a vanadium-doped polyacrylic acid foam target shot, detailed modeling was attempted. The spectral flux was determined with data from 5 XRD channels and deconvolved using the code SHAZAM. The observed decay in reflectivity was assumed to correspond to the melting of the first tungsten layer. A ''conduction factor'' of 82 was required to manipulate the heat loading of the first tungsten layer such that the time of melting corresponded to the observed decay. The power at destruction was 141 MW/cm/sup 2/ and the integrated energy at destruction was 2.0 J/cm/sup 2/. 82 refs., 66 figs., 10 tabs.

  19. X-ray Spectral Variation of Eta Carinae through the 2003 X-ray Minimum

    OpenAIRE

    Hamaguchi, Kenji; Corcoran, Michael F.; Gull, Theodore; Ishibashi, Kazunori; Pittard, Julian M.; Hillier, D. John; Damineli, Augusto; Davidson, Kris; Nielsen, Krister E.; Kober, Gladys Vieira

    2007-01-01

    We report the results of an X-ray observing campaign on the massive, evolved star Eta Carinae, concentrating on the 2003 X-ray minimum as seen by the XMM-Newton observatory. These are the first spatially-resolved X-ray monitoring observations of the stellar X-ray spectrum during the minimum. The hard X-ray emission, believed to be associated with the collision of Eta Carinae's wind with the wind from a massive companion star, varied strongly in flux on timescales of days, but not significantl...

  20. Large area soft x-ray collimator to facilitate x-ray optics testing

    Science.gov (United States)

    Espy, Samuel L.

    1994-01-01

    The first objective of this program is to design a nested conical foil x-ray optic which will collimate x-rays diverging from a point source. The collimator could then be employed in a small, inexpensive x-ray test stand which would be used to test various x-ray optics and detector systems. The second objective is to demonstrate the fabrication of the x-ray reflectors for this optic using lacquer-smoothing and zero-stress electroforming techniques.

  1. First X-ray fluorescence CT experimental results at the SSRF X-ray imaging beamline

    Institute of Scientific and Technical Information of China (English)

    DENG Biao; YANG Qun; XIE Hong-Lan; DU Guo-Hao; XIAO Wi-Qiao

    2011-01-01

    X-ray fluorescence CT is a non-destructive technique for detecting elemental composition and distribution inside a specimen. In this paper, the first experimental results of X-ray fluorescence CT obtained at the SSRF X-ray imaging beamline (BL13W1) are described. The test samples were investigated and the 2D elemental image was reconstructed using a filtered back-projection algorithm. In the sample the element Cd was observed. Up to now, the X-ray fluorescence CT could be carried out at the SSRF X-ray imaging beamline.

  2. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    OpenAIRE

    Miaja-Avila, L.; G. C. O'Neil; Uhlig, J.; C. L. Cromer; Dowell, M. L.; Jimenez, R.; Hoover, A. S.; Silverman, K. L.; Ullom, J. N.

    2015-01-01

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼106 photons/s, by focusing the produced x-rays with a polycapillary opti...

  3. Using Two-Dimensional Colloidal Crystals to Understand Crystallography

    Science.gov (United States)

    Bosse, Stephanie A.; Loening, Nikolaus M.

    2008-01-01

    X-ray crystallography is an essential technique for modern chemistry and biochemistry, but it is infrequently encountered by undergraduate students owing to lack of access to equipment, the time-scale for generating diffraction-quality molecular crystals, and the level of mathematics involved in analyzing the resulting diffraction patterns.…

  4. Dual-energy X-ray CT and the extension to polychromatic X-ray CT

    International Nuclear Information System (INIS)

    We have developed dual energy X-ray CT using monochromatic X-ray beams. From the dual-energy X-ray CT, we can obtain distributions of an electron density and an effective atomic number in a human body. Especially, the electron density is very important for the heavy ion radiotherapy. Now, we adopted new array-detector to know the energy of incident photons as well as detect the position and the number of photons. We carry out the experiment of the dual-energy X-ray CT at the beamline of KEK and SPring-8 as a fundamental study for the polychromatic X-ray CT. We will show the preliminary result of this experiments and the feasibility of a quantitative polychromatic X-ray CT as an advanced method of monochromatic X-ray CT in this study. (author)

  5. Three-dimensional imaging of nanoscale materials by using coherent x-rays

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Jianwei

    2011-04-18

    X-ray crystallography is currently the primary methodology used to determine the 3D structure of materials and macromolecules. However, many nanostructures, disordered materials, biomaterials, hybrid materials and biological specimens are noncrystalline and, hence, their structures are not accessible by X-ray crystallography. Probing these structures therefore requires the employment of different approaches. A very promising technique currently under rapid development is X-ray diffraction microscopy (or lensless imaging), in which the coherent X-ray diffraction pattern of a noncrystalline specimen is measured and then directly phased to obtain a high-resolution image. Through the DOE support over the past three years, we have applied X-ray diffraction microscopy to quantitative imaging of GaN quantum dot particles, and revealed the internal GaN-Ga2O3 core shell structure in three dimensions. By exploiting the abrupt change in the scattering cross-section near electronic resonances, we carried out the first experimental demonstration of resonant X-ray diffraction microscopy for element specific imaging. We performed nondestructive and quantitative imaging of buried Bi structures inside a Si crystal by directly phasing coherent X-ray diffraction patterns acquired below and above the Bi M5 edge. We have also applied X-ray diffraction microscopy to nondestructive imaging of mineral crystals inside biological composite materials - intramuscular fish bone - at the nanometer scale resolution. We identified mineral crystals in collagen fibrils at different stages of mineralization and proposed a dynamic mechanism to account for the nucleation and growth of mineral crystals in the collagen matrix. In addition, we have also discovered a novel 3D imaging modality, denoted ankylography, which allows for complete 3D structure determination without the necessity of sample titling or scanning. We showed that when the diffraction pattern of a finite object is sampled at a

  6. Cell survival studies using ultrasoft x rays

    International Nuclear Information System (INIS)

    Cell survival was studied for V79 hamster, 10T1/2 mouse, and human skin fibroblast cell lines, using carbon K (0.28 keV), copper K (8.0 keV), and 250 kVp x rays. Because of the rapid attenuation of the carbon x rays, cellular dimensions at the time of exposure were measured using optical and electron microscopy, and frequency distributions of mean dose absorbed by the cell nucleus were obtained. The results indicate that the differences in cell killing between ultra-soft and hard x rays may depend on the nuclear thickness of the cells. Studies of the effects of hypoxia on V79 and 10T1/2 cells using carbon K, aluminum K (1.5 keV), and copper K x rays show decreasing OER values with decreasing x-ray energy and no difference between the two cell lines. Age response studies with V79 cells show similar cell-cycle variation of survival for carbon K and aluminum K x rays as for hard x rays

  7. Toward Adaptive X-Ray Telescopes

    Science.gov (United States)

    O'Dell, Stephen L.; Atkins, Carolyn; Button, Tim W.; Cotroneo, Vincenzo; Davis, William N.; Doel, Peer; Feldman, Charlotte H.; Freeman, Mark D.; Gubarev, Mikhail V.; Kolodziejczak, Jeffrey J.; Michette, Alan G.; Ramsey, Brian D.; Reid, Paul B.; Rodriguez Sanmartin, Daniel; Saha, Timo T.; Schwartz, Daniel A.; Trolier-McKinstry, Susan; Wilke, Rudeger H. T.; Willingale, Richard; Zhang, William W.

    2011-01-01

    Future x-ray observatories will require high-resolution (less than 1 inch) optics with very-large-aperture (greater than 25 square meter) areas. Even with the next generation of heavy-lift launch vehicles, launch-mass constraints and aperture-area requirements will limit the surface areal density of the grazing-incidence mirrors to about 1 kilogram per square meter or less. Achieving sub-arcsecond x-ray imaging with such lightweight mirrors will require excellent mirror surfaces, precise and stable alignment, and exceptional stiffness or deformation compensation. Attaining and maintaining alignment and figure control will likely involve adaptive (in-space adjustable) x-ray optics. In contrast with infrared and visible astronomy, adaptive optics for x-ray astronomy is in its infancy. In the middle of the past decade, two efforts began to advance technologies for adaptive x-ray telescopes: The Generation-X (Gen-X) concept studies in the United States, and the Smart X-ray Optics (SXO) Basic Technology project in the United Kingdom. This paper discusses relevant technological issues and summarizes progress toward adaptive x-ray telescopes.

  8. Toward active x-ray telescopes

    Science.gov (United States)

    O'Dell, Stephen L.; Atkins, Carolyn; Button, Timothy W.; Cotroneo, Vincenzo; Davis, William N.; Doel, Peter; Feldman, Charlotte H.; Freeman, Mark D.; Gubarev, Mikhail V.; Kolodziejczak, Jeffery J.; Michette, Alan G.; Ramsey, Brian D.; Reid, Paul B.; Rodriguez Sanmartin, Daniel; Saha, Timo T.; Schwartz, Daniel A.; Trolier-McKinstry, Susan; Wilke, Rudeger H. T.; Willingale, Richard; Zhang, William W.

    2011-09-01

    Future x-ray observatories will require high-resolution ( 25 m2) areas. Even with the next generation of heavy-lift launch vehicles, launch-mass constraints and aperture-area requirements will limit the areal density of the grazing-incidence mirrors to about 1 kg/m2 or less. Achieving sub-arcsecond x-ray imaging with such lightweight mirrors will require excellent mirror surfaces, precise and stable alignment, and exceptional stiffness or deformation compensation. Attaining and maintaining alignment and figure control will likely involve active (in-space adjustable) x-ray optics. In contrast with infrared and visible astronomy, active optics for x-ray astronomy is in its infancy. In the middle of the past decade, two efforts began to advance technologies for adaptive x-ray telescopes: The Smart X-ray Optics (SXO) Basic Technology project in the United Kingdom (UK) and the Generation-X (Gen-X) concept studies in the United States (US). This paper discusses relevant technological issues and summarizes progress toward active x-ray telescopes.

  9. Characterizing automotive fuel cell materials by soft x-ray scanning transmission x-ray microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hitchcock, A. P., E-mail: aph@mcmaster.ca; Lee, V.; Wu, J.; Cooper, G. [Chemistry & Chemical Biology, McMaster University, Hamilton, ON, L8S 4M1 (Canada); West, M. M.; Berejnov, V. [Faculty of Health Sciences Electron Microscopy, McMaster University, Hamilton, ON L8N 3Z5 (Canada); Soboleva, T.; Susac, D.; Stumper, J. [Automotive Fuel Cell Cooperation Corp., Burnaby BC V5J 5J8 (Canada)

    2016-01-28

    Proton-Exchange Membrane Fuel Cell (PEM-FC) based engines are being developed rapidly for near-term implementation in hydrogen fueled, mass production, personal automobiles. Research is focused on understanding and controlling various degradation processes (carbon corrosion, Pt migration, cold start), and reducing cost by reducing or eliminating Pt catalyst. We are using soft X-ray scanning transmission X-ray microscopy (STXM) at the S 2p, C 1s, O 1s and F 1s edges to study a variety of issues related to optimization of PEM-FC materials for automotive applications. A method to efficiently and accurately measure perfluorosulfonic acid distributions was developed and is being used to better understand how different loadings and preparation methods affect the ionomer distribution in the cathode. Progress towards an environmental cell capable of controlling the temperature and humidity of a PEM-FC sample in the STXM is described. Methods for studying the 3D chemical structure of PEM-FC are outlined.

  10. Characterizing automotive fuel cell materials by soft x-ray scanning transmission x-ray microscopy

    International Nuclear Information System (INIS)

    Proton-Exchange Membrane Fuel Cell (PEM-FC) based engines are being developed rapidly for near-term implementation in hydrogen fueled, mass production, personal automobiles. Research is focused on understanding and controlling various degradation processes (carbon corrosion, Pt migration, cold start), and reducing cost by reducing or eliminating Pt catalyst. We are using soft X-ray scanning transmission X-ray microscopy (STXM) at the S 2p, C 1s, O 1s and F 1s edges to study a variety of issues related to optimization of PEM-FC materials for automotive applications. A method to efficiently and accurately measure perfluorosulfonic acid distributions was developed and is being used to better understand how different loadings and preparation methods affect the ionomer distribution in the cathode. Progress towards an environmental cell capable of controlling the temperature and humidity of a PEM-FC sample in the STXM is described. Methods for studying the 3D chemical structure of PEM-FC are outlined

  11. Characterizing automotive fuel cell materials by soft x-ray scanning transmission x-ray microscopy

    Science.gov (United States)

    Hitchcock, A. P.; Lee, V.; Wu, J.; West, M. M.; Cooper, G.; Berejnov, V.; Soboleva, T.; Susac, D.; Stumper, J.

    2016-01-01

    Proton-Exchange Membrane Fuel Cell (PEM-FC) based engines are being developed rapidly for near-term implementation in hydrogen fueled, mass production, personal automobiles. Research is focused on understanding and controlling various degradation processes (carbon corrosion, Pt migration, cold start), and reducing cost by reducing or eliminating Pt catalyst. We are using soft X-ray scanning transmission X-ray microscopy (STXM) at the S 2p, C 1s, O 1s and F 1s edges to study a variety of issues related to optimization of PEM-FC materials for automotive applications. A method to efficiently and accurately measure perfluorosulfonic acid distributions was developed and is being used to better understand how different loadings and preparation methods affect the ionomer distribution in the cathode. Progress towards an environmental cell capable of controlling the temperature and humidity of a PEM-FC sample in the STXM is described. Methods for studying the 3D chemical structure of PEM-FC are outlined.

  12. Adsorption and deposition of anthraquinone-2-carboxylic acid on alumina studied by inelastic electron tunneling spectroscopy, infrared reflection absorption spectroscopy, X-ray photoelectron spectroscopy, and atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Higo, Morihide [Department of Applied Chemistry and Chemical Engineering, Faculty of Engineering, Kagoshima University, 1-21-40 Korimoto, Kagoshima 890-0065 (Japan)], E-mail: higo@apc.kagoshima-u.ac.jp; Miake, Takeshi; Mitsushio, Masaru; Yoshidome, Toshifumi [Department of Applied Chemistry and Chemical Engineering, Faculty of Engineering, Kagoshima University, 1-21-40 Korimoto, Kagoshima 890-0065 (Japan); Ozono, Yoshihisa [Center for Instrumental analysis, Kagoshima University, 1-21-40 Korimoto, Kagoshima 890-0065 (Japan)

    2008-04-30

    The adsorption state of anthraquinone-2-carboxylic acid (AQ-2-COOH) deposited from acetone solutions (0.01-1.00 mg/ml) on native oxide surfaces of Al films was characterized by inelastic electron tunneling spectroscopy, infrared reflection absorption spectroscopy, and X-ray photoelectron spectroscopy. The oxide was prepared on evaporated Al films at room temperature in an oxygen-dc glow discharge. The morphology of the deposited AQ-2-COOH on the oxide surfaces was observed and analyzed by atomic force microscopy. These surface analyses showed that AQ-2-COOH is adsorbed predominantly as a uniform nanometer-scale film of carboxylate anions on the oxide surfaces deposited from solutions with concentrations lower than or equal to 0.02 mg/ml. It was found that AQ-2-COOH is adsorbed as both a uniform film of anions and as micron-sized particles of neutral molecules with heights of a few tens of nanometers when AQ-2-COOH is deposited from solutions with concentrations higher than 0.02 mg/ml. A comparison of the results obtained by these surface analytical techniques clearly shows the features and advantages of these analytical techniques.

  13. Adsorption and deposition of anthraquinone-2-carboxylic acid on alumina studied by inelastic electron tunneling spectroscopy, infrared reflection absorption spectroscopy, X-ray photoelectron spectroscopy, and atomic force microscopy

    International Nuclear Information System (INIS)

    The adsorption state of anthraquinone-2-carboxylic acid (AQ-2-COOH) deposited from acetone solutions (0.01-1.00 mg/ml) on native oxide surfaces of Al films was characterized by inelastic electron tunneling spectroscopy, infrared reflection absorption spectroscopy, and X-ray photoelectron spectroscopy. The oxide was prepared on evaporated Al films at room temperature in an oxygen-dc glow discharge. The morphology of the deposited AQ-2-COOH on the oxide surfaces was observed and analyzed by atomic force microscopy. These surface analyses showed that AQ-2-COOH is adsorbed predominantly as a uniform nanometer-scale film of carboxylate anions on the oxide surfaces deposited from solutions with concentrations lower than or equal to 0.02 mg/ml. It was found that AQ-2-COOH is adsorbed as both a uniform film of anions and as micron-sized particles of neutral molecules with heights of a few tens of nanometers when AQ-2-COOH is deposited from solutions with concentrations higher than 0.02 mg/ml. A comparison of the results obtained by these surface analytical techniques clearly shows the features and advantages of these analytical techniques

  14. Neutralization of calcite in mineral aerosols by acidic sullur species collected in China and Japan studied by ca K-edge X-ray absorption near-edge structure.

    Science.gov (United States)

    Takahashi, Yoshio; Miyoshi, Takuro; Higashi, Masayuki; Kamioka, Hikari; Kanai, Yutaka

    2009-09-01

    Calcium species in mineral aerosols collected simultaneously in Aksu (near the Taklimakan Desert), Qingdao (eastern China), and Tsukuba (Japan) during dust and nondust periods were determined using Ca K-edge X-ray absorption near-edge structure (XANES). From the fitting of XANES spectra, it was found that (i) calcite and gypsum were the main Ca species in the aerosol samples, and (ii) the gypsum fraction versus total Ca minerals [Gyp]/[Ca2+]t increased progressively in the order Aksu aerosols for all the samples except for that taken in Aksu during the dust period. The decrease of the [Gyp]/[Ca2+]t ratio with an increase in particle size showed that the neutralization effect proceeds from the particle surface. For the Aksu sample in the dust period, however, (i) the [Gyp]/[Ca2+]t ratios obtained by XANES measured in the fluorescence (FL; regarded as bulk analysis) and CEY modes were similar and (ii) size dependence was not found, showing that neutralization is not important for the sample because of the large supply of mineral aerosol with little neutralization effect in Aksu. It was also found that the pH of the aerosol and the ratio of (NH4)2SO4 to gypsum were positively and negatively correlated with the Ca (or calcite) content, respectively. The speciation of Ca by XANES revealed the neutralization processes of acidic sulfur species by calcite during the long-range transport of mineral aerosols. PMID:19764213

  15. Two-dimensional x-ray diffraction

    CERN Document Server

    He, Bob B

    2009-01-01

    Written by one of the pioneers of 2D X-Ray Diffraction, this useful guide covers the fundamentals, experimental methods and applications of two-dimensional x-ray diffraction, including geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis and combinatorial screening. Experimental examples in materials research, pharmaceuticals, and forensics are also given. This presents a key resource to resea

  16. Imaging Cellular Architecture with X-rays

    OpenAIRE

    Larabell, Carolyn A.; Nugent, Keith A.

    2010-01-01

    X-ray imaging of biological samples is progressing rapidly. In this paper we review the progress to date in high resolution imaging of cellular architecture. In particular we survey the progress in soft X-ray tomography and argue that the field is coming of age and that important biological insights are starting to emerge. We then review the new ideas based on coherent diffraction. These methods are at a much earlier stage of development but, as they eliminate the need for X-ray optics, have ...

  17. The Future of X-Ray Optics

    Science.gov (United States)

    Weisskopf, Martin C.

    2013-01-01

    The most important next step is the development of X-ray optics comparable to (or better than) Chandra in angular resolution that far exceed Chandra s effective area. Use the long delay to establish an adequately funded, competitive technology program along the lines I have recommended. Don't be diverted from this objective, except for Explorer-class missions. Progress in X-ray optics, with emphasis on the angular resolution, is central to the paradigm-shifting discoveries and the contributions of X-ray astronomy to multiwavelength astrophysics over the past 51 years.

  18. Ten years of X-ray interferometry

    International Nuclear Information System (INIS)

    X-ray interferometers were the first optical instruments which utilized many Bragg reflecting components in monolithic blocks of perfect crystal. They have made important contributions to our knowledge of fundamental constants, of Bragg reflection x-ray optics, of strains and defects in crystals and of the optical constants of materials in the x-ray region of the electromagnetic spectrum. Based on an oversimplified optical analogue, their mode of operation is described in detail. Current applications of crystal interferometers and future work is briefly reviewed. (author)

  19. X-ray phase-contrast methods

    Energy Technology Data Exchange (ETDEWEB)

    Lider, V. V., E-mail: lider@ns.crys.ras.ru; Kovalchuk, M. V. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2013-11-15

    This review is devoted to a comparative description of the methods for forming X-ray phase-contrast images of weakly absorbing (phase) objects. These include the crystal interferometer method, the Talbot interferometer method, diffraction-enhanced X-ray imaging, and the in-line method. The potential of their practical application in various fields of science and technology is discussed. The publications on the development and optimization of X-ray phase-contrast methods and the experimental study of phase objects are analyzed.

  20. Microfabrication of hard x-ray lenses

    DEFF Research Database (Denmark)

    Stöhr, Frederik

    in the vertical and horizontal directions was addressed. A functioning prototype of a 2D silicon objective for use in a bright-field hard-XRM was demonstrated. The results are promising; showing acceptably low aberration and performance close to theoretical expectations. A resolution of 300 nm with 17 keV x...... rate larger than 10 pieces per hour indicates the economic value of injection molded x-ray lenses, which may have applications in more readily available small laboratory x-ray instruments or medical devices. In each case, observed non-uniformities of the shaped x-ray beams were investigated and found...

  1. Protein Energy Landscapes Determined by 5-Dimensional Crystallography

    CERN Document Server

    Schmidt, Marius; Henning, Robert; Ihee, Hyotcherl; Purwar, Namrta; Tenboer, Jason; Tripathi, Shailesh

    2013-01-01

    Free energy landscapes decisively determine the progress of enzymatically catalyzed reactions[1]. Time-resolved macromolecular crystallography unifies transient-state kinetics with structure determination [2-4] because both can be determined from the same set of X-ray data. We demonstrate here how barriers of activation can be determined solely from five-dimensional crystallography [5]. Directly linking molecular structures with barriers of activation between them allows for gaining insight into the structural nature of the barrier. We analyze comprehensive time series of crystal-lographic data at 14 different temperature settings and determine entropy and enthalpy contributions to the barriers of activation. 100 years after the discovery of X-ray scattering, we advance X-ray structure determination to a new frontier, the determination of energy landscapes.

  2. Structural changes caused by radiation-induced reduction and radiolysis: the effect of X-ray absorbed dose in a fungal multicopper oxidase

    Energy Technology Data Exchange (ETDEWEB)

    De la Mora, Eugenio [Universidad Nacional Autónoma de México, Avenida Universidad 2001, Cuernavaca, Morelos 62210 (Mexico); Lovett, Janet E. [University of Oxford, South Parks Road, Oxford OX1 3QR (United Kingdom); University of Oxford, South Parks Road, Oxford OX1 3RE (United Kingdom); EaStCHEM School of Chemistry, Joseph Black Building, The King’s Buildings, Edinburgh EH9 3JJ, Scotland (United Kingdom); Blanford, Christopher F. [University of Oxford, South Parks Road, Oxford OX1 3QR (United Kingdom); Manchester Interdisciplinary Biocentre, 131 Princess Street, Manchester M1 7DN (United Kingdom); Garman, Elspeth F. [University of Oxford, South Parks Road, Oxford OX1 3QU (United Kingdom); Valderrama, Brenda; Rudino-Pinera, Enrique, E-mail: rudino@ibt.unam.mx [Universidad Nacional Autónoma de México, Avenida Universidad 2001, Cuernavaca, Morelos 62210 (Mexico)

    2012-05-01

    Radiation-induced reduction, radiolysis of copper sites and the effect of pH value together with the concomitant geometrical distortions of the active centres were analysed in several fungal (C. gallica) laccase structures collected at cryotemperature. This study emphasizes the importance of careful interpretation when the crystallographic structure of a metalloprotein is described. X-ray radiation induces two main effects at metal centres contained in protein crystals: radiation-induced reduction and radiolysis and a resulting decrease in metal occupancy. In blue multicopper oxidases (BMCOs), the geometry of the active centres and the metal-to-ligand distances change depending on the oxidation states of the Cu atoms, suggesting that these alterations are catalytically relevant to the binding, activation and reduction of O{sub 2}. In this work, the X-ray-determined three-dimensional structure of laccase from the basidiomycete Coriolopsis gallica (Cg L), a high catalytic potential BMCO, is described. By combining spectroscopic techniques (UV–Vis, EPR and XAS) and X-ray crystallography, structural changes at and around the active copper centres were related to pH and absorbed X-ray dose (energy deposited per unit mass). Depletion of two of the four active Cu atoms as well as low occupancies of the remaining Cu atoms, together with different conformations of the metal centres, were observed at both acidic pH and high absorbed dose, correlating with more reduced states of the active coppers. These observations provide additional evidence to support the role of flexibility of copper sites during O{sub 2} reduction. This study supports previous observations indicating that interpretations regarding redox state and metal coordination need to take radiation effects explicitly into account.

  3. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy.

    Science.gov (United States)

    Miaja-Avila, L; O'Neil, G C; Uhlig, J; Cromer, C L; Dowell, M L; Jimenez, R; Hoover, A S; Silverman, K L; Ullom, J N

    2015-03-01

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼10(6) photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >10(7) laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  4. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    Directory of Open Access Journals (Sweden)

    L. Miaja-Avila

    2015-03-01

    Full Text Available We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  5. Recent Developments of Multilayer Mirror Optics for Laboratory X-ray Instrumentation

    Science.gov (United States)

    Michaelsen, Carsten; Wiesmann, Jörg; Hoffmann, C.; Wulf, K.; Brugemann, Lutz; Storm, A.

    2002-12-01

    In this paper we review various improvements that we made in the development of multilayer mirror optics for home-lab x-ray analytical equipment in recent years. For the detection of light elements using x-ray fluorescence spectrometry, we developed a number of new multilayers with improved detection limits. In detail, we found that La/B4C multilayers improve the detection limit of boron by 29 % compared to the previous Mo/B4C multilayers. For the detection of carbon, TiO2/C multilayers improve the detection limit also by 29 % compared to the V/C multilayers previously used. For the detection of aluminum, WSi2/Si or Ta/Si multilayers can lead to detection limit improvements over the current W/Si multilayers of up to 60 % for samples on silicon wafers. For the use as beam-conditioning elements in x-ray diffractometry, curved optics coated with laterally d-spacing graded multilayers give rise to major improvements concerning usable x-ray intensity and beam quality. Recent developments lead to a high quality of these multilayer optics concerning beam intensity, divergence, beam uniformity and spectral purity. For example, x-ray reflectometry instruments equipped with such multilayer optics have dynamic ranges previously only available at synchrotron sources. Two-dimensional focusing multilayer optics are shown to become essential optical elements in protein crystallography and structural proteomics.

  6. X-ray diffraction contrast tomography (DCT) system, and an X-ray diffraction contrast tomography (DCT) method

    DEFF Research Database (Denmark)

    2012-01-01

    Source: US2012008736A An X-ray diffraction contrast tomography system (DCT) comprising a laboratory X-ray source (2), a staging device (5) rotating a polycrystalline material sample in the direct path of the X-ray beam, a first X-ray detector (6) detecting the direct X-ray beam being transmitted...

  7. Future X-ray timing missions

    CERN Document Server

    Barret, D; Staubert, R; Stella, L

    2000-01-01

    Thanks to the Rossi X-ray Timing Explorer (RXTE), it is now widely recognized that fast X-ray timing can be used to probe strong gravity fields around collapsed objects and constrain the equation of state of dense matter in neutron stars. We first discuss some of the outstanding issues which could be solved with an X-ray timing mission building on the great successes of RXTE and providing an order of magnitude better sensitivity. Then we briefly describe the 'Experiment for X-ray timing and Relativistic Astrophysics' (EXTRA) recently proposed to the European Space Agency as a follow-up to RXTE and the related US mission 'Relativistic Astrophysics Explorer' (RAE).

  8. Future X-Ray Timing Missions

    Science.gov (United States)

    Barret, Didier; van der Klis, Michiel; Skinner, Gerry K.; Staubert, Rüdiger; Stella, Luigi

    Thanks to the Rossi X-ray Timing Explorer (RXTE), it is now widely recognized that fast X-ray timing can be used to probe strong gravity fields around collapsed objects and constrain the equation of state of dense matter in neutron stars. We first discuss some of the outstanding issues which could be solved with an X-ray timing mission building on the great successes of RXTE and providing an order of magnitude better sensitivity. Then we briefly describe the `Experiment for X-ray timing and Relativistic Astrophysics' (EXTRA) recently proposed to the European Space Agency as a follow-up to RXTE and the related US mission `Relativistic Astrophysics Explorer' (RAE).

  9. Experimental x-ray ghost imaging

    CERN Document Server

    Pelliccia, Daniele; Scheel, Mario; Cantelli, Valentina; Paganin, David M

    2016-01-01

    We report an experimental proof of principle for ghost imaging in the hard x-ray energy range. We used a synchrotron x-ray beam that was split using a thin crystal in Laue diffraction geometry. With an ultra-fast imaging camera, we were able to image x-rays generated by isolated electron bunches. At this time scale, the shot noise of the synchrotron emission process is measurable as speckles, leading to speckle correlation between the two beams. The integrated transmitted intensity from a sample located in the first beam was correlated with the spatially resolved intensity measured on the second, empty, beam to retrieve the shadow of the sample. The demonstration of ghost imaging with hard x-rays may open the way to protocols to reduce radiation damage in medical imaging and in non-destructive structural characterization using Free Electron Lasers.

  10. Experimental X-Ray Ghost Imaging

    Science.gov (United States)

    Pelliccia, Daniele; Rack, Alexander; Scheel, Mario; Cantelli, Valentina; Paganin, David M.

    2016-09-01

    We report an experimental proof of principle for ghost imaging in the hard-x-ray energy range. We use a synchrotron x-ray beam that is split using a thin crystal in Laue diffraction geometry. With an ultrafast imaging camera, we are able to image x rays generated by isolated electron bunches. At this time scale, the shot noise of the synchrotron emission process is measurable as speckles, leading to speckle correlation between the two beams. The integrated transmitted intensity from a sample located in the first beam is correlated with the spatially resolved intensity measured in the second, empty, beam to retrieve the shadow of the sample. The demonstration of ghost imaging with hard x rays may open the way to protocols to reduce radiation damage in medical imaging and in nondestructive structural characterization using free electron lasers.

  11. Center for X-ray Optics (CXRO)

    Data.gov (United States)

    Federal Laboratory Consortium — The Center for X-Ray Optics at Lawrence Berkeley National Laboratory works to further science and technology using short wavelength optical systems and techniques....

  12. Why Do I Need X-Rays?

    Science.gov (United States)

    ... information you need from the Academy of General Dentistry Wednesday, August 24, 2016 About | Contact InfoBites Quick ... Related Articles: X-Rays The Academy of General Dentistry (AGD) Sets the Record Straight on Dental X- ...

  13. X-Ray Technologist Listing In California

    Data.gov (United States)

    U.S. Department of Health & Human Services — This table represents a current listing of X-Ray Technologists who are licensed by Radiologic Health Branch (RHB) of the California Department of Public Health. RHB...

  14. X-ray source for mammography

    Science.gov (United States)

    Logan, Clinton M.

    1994-01-01

    An x-ray source utilizing anode material which shifts the output spectrum to higher energy and thereby obtains higher penetrating ability for screening mammography application, than the currently utilized anode material. The currently used anode material (molybdenum) produces an energy x-ray spectrum of 17.5/19.6 keV, which using the anode material of this invention (e.g. silver, rhodium, and tungsten) the x-ray spectrum would be in the 20-35 keV region. Thus, the anode material of this invention provides for imaging of breasts with higher than average x-ray opacity without increase of the radiation dose, and thus reduces the risk of induced breast cancer due to the radiation dose administered for mammograms.

  15. Tuberculosis, advanced - chest x-rays (image)

    Science.gov (United States)

    Tuberculosis is an infectious disease that causes inflammation, the formation of tubercules and other growths within tissue, ... death. These chest x-rays show advanced pulmonary tuberculosis. There are multiple light areas (opacities) of varying ...

  16. Chest X-Ray (Chest Radiography)

    Science.gov (United States)

    ... Lung tissue absorbs little radiation and will appear dark on the image. Until recently, x-ray images ... understanding of the possible charges you will incur. Web page review process: This Web page is reviewed ...

  17. X-ray microtomography in biology

    CERN Document Server

    Mizutani, Ryuta

    2016-01-01

    Progress in high-resolution x-ray microtomography has provided us with a practical approach to determining three-dimensional (3D) structures of opaque samples at micrometer to submicrometer resolution. In this review, we give an introduction to hard x-ray microtomography and its application to the visualization of 3D structures of biological soft tissues. Practical aspects of sample preparation, handling, data collection, 3D reconstruction, and structure analysis are described. Furthermore, different sample contrasting methods are approached in detail. Examples of microtomographic studies are overviewed to present an outline of biological applications of x-ray microtomography. We also provide perspectives of biological microtomography as the convergence of sciences in x-ray optics, biology, and structural analysis.

  18. X-ray imaging: Status and trends

    International Nuclear Information System (INIS)

    There is a veritable renaissance occurring in x-ray imaging. X-ray imaging by radiography has been a highly developed technology in medicine and industry for many years. However, high resolution imaging has not generally been practical because sources have been relatively dim and diffuse, optical elements have been nonexistent for most applications, and detectors have been slow and of low resolution. Materials analysis needs have therefore gone unmet. Rapid progress is now taking place because we are able to exploit developments in microelectronics and related material fabrication techniques, and because of the availability of intense x-ray sources. This report describes the methods and uses of x-ray imaging along with a discussion of technology advances in these areas

  19. 5.8 X-ray Calorimeters

    Science.gov (United States)

    Porter, F. Scott

    2008-01-01

    X-ray calorimeter instruments for astrophysics have seen rapid development since they were invented in 1984. The prime instrument on all currently planned X-ray spectroscopic observatories is based on calorimeter technology. This relatively simple detection concept that senses the energy of an incident photon by measuring the temperature rise of an absorber material at very low temperatures, can form the basis of a very high performance, non-dispersive spectrometer. State-of-the-art calorimeter instruments have resolving powers of over 3000, large simultaneous band-passes, and near unit efficiency. This coupled with the intrinsic imaging capability of a pixilated x-ray calorimeter array, allows true spectral-spatial instruments to be constructed. In this chapter I briefly review the detection scheme, the state-of-the-art in X-ray calorimeter instruments and the future outlook for this technology.

  20. Silicon Wafer X-ray Mirror Project

    Data.gov (United States)

    National Aeronautics and Space Administration — In this one year research project, we propose to do the following four tasks; (1) Design the silicon wafer X-ray mirror demo unit and develop a ray-tracing code to...

  1. Silicon Wafer X-ray Mirror Project

    Data.gov (United States)

    National Aeronautics and Space Administration — In this one year research project, we propose to do the following four tasks;(1) Design the silicon wafer X-ray mirror demo unit and develop a ray-tracing code to...

  2. Dental x-ray diagnostic installation

    International Nuclear Information System (INIS)

    An exemplary embodiment comprises an exposure unit including an X-ray tube and a cassette holder rotatable about vertical axes and between which the head of the patient is disposed. A radiation detector is disposed at the cassette holder for supplying an electrical signal corresponding to the dose rate when it is struck by X-rays and being interconnected with an X-ray tube voltage controller and a dose rate regulator in such manner that the X-ray tube voltage is influenced by the output of the radiation detector to control the dose rate to a value producing an optimum film blackening. A function generator determining the speed of the exposure unit is provided in which a speed curve is stored given which the radiation dose influencing the film is approximately constant

  3. Demonstration of X-ray talbot interferometry

    CERN Document Server

    Momose, A; Kawamoto, S; Hamaishi, Y; Takai, K; Suzuki, Y

    2003-01-01

    First Talbot interferometry in the hard X-ray region was demonstrated using a pair of transmission gratings made by forming gold stripes on glass plates. By aligning the gratings on the optical axis of X-rays with a separation that caused the Talbot effect by the first grating, moire fringes were produced inclining one grating slightly against the other around the optical axis. A phase object placed in front of the first grating was detected by moire-fringe bending. Using the technique of phase-shifting interferometry, the differential phase corresponding to the phase object could also be measured. This result suggests that X-ray Talbot interferometry is a novel and simple method for phase-sensitive X-ray radiography. (author)

  4. Resonant X-Ray Scattering and Absorption

    Science.gov (United States)

    Collins, S. P.; Bombardi, A.

    This chapter outlines some of the basic ideas behind nonresonant and resonant X-ray scattering, using classical or semiclassical pictures wherever possible; specifically, we highlight symmetry arguments governing the observation of X-ray optical effects, such as X-ray magnetic circular dichroism and resonant "forbidden" diffraction. Without dwelling on the microscopic physics that underlies resonant scattering, we outline some key steps required for calculating its rotation and polarization dependence, based on Cartesian and spherical tensor frameworks. Several examples of resonant scattering, involving electronic anisotropy and magnetism, are given as illustrations. Our goal is not to develop or defend theoretical concepts in X-ray scattering, but to bring together existing ideas in a pragmatic and utilitarian manner.

  5. Nonrelativistic quantum X-ray physics

    CERN Document Server

    Hau-Riege, Stefan P

    2015-01-01

    Providing a solid theoretical background in photon-matter interaction, Nonrelativistic Quantum X-Ray Physics enables readers to understand experiments performed at XFEL-facilities and x-ray synchrotrons. As a result, after reading this book, scientists and students will be able to outline and perform calculations of some important x-ray-matter interaction processes. Key features of the contents are that the scope reaches beyond the dipole approximation when necessary and that it includes short-pulse interactions. To aid the reader in this transition, some relevant examples are discussed in detail, while non-relativistic quantum electrodynamics help readers to obtain an in-depth understanding of the formalisms and processes. The text presupposes a basic (undergraduate-level) understanding of mechanics, electrodynamics, and quantum mechanics. However, more specialized concepts in these fields are introduced and the reader is directed to appropriate references. While primarily benefiting users of x-ray light-sou...

  6. Astrophysics: Unexpected X-ray flares

    Science.gov (United States)

    Campana, Sergio

    2016-10-01

    Two sources of highly energetic flares have been discovered in archival X-ray data of 70 nearby galaxies. These flares have an undetermined origin and might represent previously unknown astrophysical phenomena. See Letter p.356

  7. Demonstration of X-ray talbot interferometry

    International Nuclear Information System (INIS)

    First Talbot interferometry in the hard X-ray region was demonstrated using a pair of transmission gratings made by forming gold stripes on glass plates. By aligning the gratings on the optical axis of X-rays with a separation that caused the Talbot effect by the first grating, moire fringes were produced inclining one grating slightly against the other around the optical axis. A phase object placed in front of the first grating was detected by moire-fringe bending. Using the technique of phase-shifting interferometry, the differential phase corresponding to the phase object could also be measured. This result suggests that X-ray Talbot interferometry is a novel and simple method for phase-sensitive X-ray radiography. (author)

  8. X-ray Emission from Solar Flares

    Indian Academy of Sciences (India)

    Rajmal Jain; Malini Aggarwal; Raghunandan Sharma

    2008-03-01

    Solar X-ray Spectrometer (SOXS), the first space-borne solar astronomy experiment of India was designed to improve our current understanding of X-ray emission from the Sun in general and solar flares in particular. SOXS mission is composed of two solid state detectors, viz., Si and CZT semiconductors capable of observing the full disk Sun in X-ray energy range of 4–56 keV. The X-ray spectra of solar flares obtained by the Si detector in the 4–25 keV range show evidence of Fe and Fe/Ni line emission and multi-thermal plasma. The evolution of the break energy point that separates the thermal and non-thermal processes reveals increase with increasing flare plasma temperature. Small scale flare activities observed by both the detectors are found to be suitable to heat the active region corona; however their location appears to be in the transition region.

  9. Inelastic magnetic X-ray scattering

    Science.gov (United States)

    Platzman, P. M.; Tzoar, N.

    1985-04-01

    The theory of magnetic X-ray scattering is used to discuss the possibilities for employing inelastic scattering to probe the magnetic properties of condensed matter systems. In particular, it is shown how the interference between the nonmagnetic (Compton) and magnetic scattering arising from the use of circularly polarized X-rays is absolutely essential in such experiments. The very beautiful preliminary experiments by Sakai and Ono (1976) on Fe which use circularly polarized Moessbauer gamma-rays will be discussed. They already show the sensitivity of the technique to the 'magnetic form factor'. In addition, the physics of a unique quarter wave plate employed in obtaining circularly polarized X-rays is considered, and the implications of this advance for doing such experiments on existing synchrotron X-ray sources are discussed.

  10. Capillary Optics generate stronger X-rays

    Science.gov (United States)

    1996-01-01

    NASA scientist, in the Space Sciences lab at Marshall, works with capillary optics that generate more intense X-rays than conventional sources. This capability is useful in studying the structure of important proteins.

  11. Insights from soft X-rays

    DEFF Research Database (Denmark)

    Raaf, Jennifer; Issinger, Olaf-Georg; Niefind, Karsten

    2008-01-01

    The diffraction pattern of a protein crystal is normally a product of the interference of electromagnetic waves scattered by electrons of the crystalline sample. The diffraction pattern undergoes systematic changes in case additionally X-ray absorption occurs, meaning if the wavelength of the pri......The diffraction pattern of a protein crystal is normally a product of the interference of electromagnetic waves scattered by electrons of the crystalline sample. The diffraction pattern undergoes systematic changes in case additionally X-ray absorption occurs, meaning if the wavelength...... of the primary X-ray beam is relatively close to the absorption edge of selected elements of the sample. The resulting effects are summarized as "anomalous dispersion" and can be always observed with "soft" X-rays (wavelength around 2 A) since they match the absorption edges of sulfur and chlorine...

  12. Dentistry 4. X-ray diagnostics

    International Nuclear Information System (INIS)

    DIN pocketbook 267/4 gives an overview of the normative requirements of the new X-Ray and Radiation Protection Ordinance, which has been in effect since 1 November 2011. This DIN pocketbook is intended for anyone charged with professional responsibility for the use of ionizing radiation in dentistry, operators and users of x-ray devices, radiation protection officers, accredited experts, manufacturers as well as for anyone with an interest in radiation protection or optimal radiological diagnostics. It contains standards relating to the following areas: acceptance and constancy testing; devices for evaluating findings (monitors, film viewing devices), films, printers; archiving, designating, labelling. Adherence to the standards makes it possible to avoid distractive artefacts in x-ray images and optimise the quality of x-ray diagnostics in dentistry.

  13. Linking Jet Emission, X-Ray States, and Hard X-Ray Tails in the Neutron Star X-Ray Binary GX 17+2

    NARCIS (Netherlands)

    S. Migliari; J.C.A. Miller-Jones; R.P. Fender; J. Homan; T. di Salvo; R.E. Rothschild; M.P. Rupen; J.A. Tomsick; R. Wijnands; M. van der Klis

    2007-01-01

    We present the results of simultaneous radio (VLA) and X-ray (RXTE) observations of the Z-type neutron star X-ray binary GX 17+2. The aim is to assess the coupling between X-ray and radio properties throughout its three rapidly variable X-ray states and during the time-resolved transitions. These ob

  14. Advanced detectors for X-ray microscopy

    International Nuclear Information System (INIS)

    Over the last decade the advances in x-ray microscopy have mainly been due to the development of x-ray source technology and to the micro-fabrication of x-ray optics. These advances have spurred the development of x-ray microscopes that are approaching the best resolution possible in the presence of radiation damage in the specimen. In addition, the development of specimen preparation techniques that reduce tile effects of radiation damage on the specimen are underway. In contrast, tile development or x-ray detectors for x-ray microscopy has been a low priority. The objective of the work was to develop a new detector for x-ray microscopy. This involved the modification of a Thorn EMI electron tube in order to sensitise the multiplier for soil x-rays In the energy range of interest (0.2-6 keV). The electron multiplier was then tested on a repetitive laser plasma source, which has been shown to be eminently suitable for a laboratory scale x-ray microscope, and the Scanning Transmission X-ray Microscope (STXM) at the National Synchrotron Light Source (NSLS), which is the most successful STXM presently in operation. The processed data from tile electron multiplier was used to characterise its response and assess its potential as all alternative to existing detectors. In addition, ID21, the microscopy beamline at the European Synchrotron Radiation Source (ESRF) was studied to assess the need for a beam position monitor close to the exit slit of the monochromator. This involved the ray tracing of the beamline. It was proposed that in the case of a crystal monochromator a beam position monitor based oil the total signal from a photo-emitting blade containing a number of different diameter pinholes was sufficient. However, for a grating monochromator tile beamline design relied upon feedback from a beam position monitor capable of detecting the height of the beam at tile entrance to the microscope. A number of conceptual designs for a monitor that could fulfil this

  15. Principles of X-ray Navigation

    Energy Technology Data Exchange (ETDEWEB)

    Hanson, John Eric; /SLAC

    2006-03-17

    X-ray navigation is a new concept in satellite navigation in which orientation, position and time are measured by observing stellar emissions in x-ray wavelengths. X-ray navigation offers the opportunity for a single instrument to be used to measure these parameters autonomously. Furthermore, this concept is not limited to missions in close proximity to the earth. X-ray navigation can be used on a variety of missions from satellites in low earth orbit to spacecraft on interplanetary missions. In 1997 the Unconventional Stellar Aspect Experiment (USA) will be launched as part of the Advanced Research and Global Observation Satellite (ARGOS). USA will provide the first platform for real-time experimentation in the field of x-ray navigation and also serves as an excellent case study for the design and manufacturing of space qualified systems in small, autonomous groups. Current techniques for determining the orientation of a satellite rely on observations of the earth, sun and stars in infrared, visible or ultraviolet wavelengths. It is possible to use x-ray imaging devices to provide arcsecond level measurement of attitude based on star patterns in the x-ray sky. This technique is explored with a simple simulation. Collimated x-ray detectors can be used on spinning satellites to provide a cheap and reliable measure of orientation. This is demonstrated using observations of the Crab Pulsar taken by the high Energy Astronomy Observatory (HEAO-1) in 1977. A single instrument concept is shown to be effective, but dependent on an a priori estimate of the guide star intensity and thus susceptible to errors in that estimate. A star scanner based on a differential measurement from two x-ray detectors eliminates the need for an a priori estimate of the guide star intensity. A first order model and a second order model of the two star scanner concepts are considered. Many of the stars that emit in the x-ray regime are also x-ray pulsars with frequency stability approaching a

  16. X-ray scattering from dense plasmas

    Energy Technology Data Exchange (ETDEWEB)

    McSherry, D.J

    2000-09-01

    Dense plasmas were studied by probing them with kilovolt x-rays and measuring those scattered at various angles. The Laser-Produced x-ray source emitted Ti He alpha 4.75 keV x-rays. Two different plasma types were explored. The first was created by laser driven shocks on either side of a sample foil consisting of 2 micron Al layer, sandwiched between two 1 micron CH layers. We have observed a peak in the x-ray scattering cross section, indicating diffraction from the plasma. However, the experimentally inferred plasma density, broadly speaking, did not always agree with the hydrodynamic simulation MEDX (A modified version of MEDUSA). The second plasma type that we studied was created by soft x-ray heating on either side of a sample foil, this time consisting of 1 micron layer of Al, sandwiched between two 0.2 micron CH layers. Two foil targets, each consisting of a 0.1 micron thick Au foil mounted on 1 micron of CH, where placed 4 mm from the sample foil. The soft x-rays where produced by laser irradiating these two foil targets. We found that, 0.5 ns after the peak of the laser heating pulses, the measured cross sections more closely matched those simulated using the Thomas Fermi model than the Inferno model. Later in time, at 2 ns, the plasma is approaching a weakly coupled state. This is the first time x-ray scattering cross sections have been measured from dense plasmas generated by radiatively heating both sides of the sample. Moreover, these are absolute values typically within a factor of two of expectation for early x-ray probe times. (author)

  17. X-ray laser program at MBI

    Science.gov (United States)

    Nickles, P. V.; Janulewicz, K. A.; Lucianetti, A.; Priebe, G.; Zigler, A.; Rocca, J. J.; Sandner, W.

    2002-11-01

    A survey of the Max Born Institute (MBI) activities in the field of X-ray lasers (XRLs) is presented. The main interest is focused on the transient soft X-ray lasers. Additionally, much work is put to look for new, efficient, compact (table-top) pumping schemes with a prospect to be applied in practice. The current state of the research and the plans for the future are described as well.

  18. Capacitor discharges, magnetohydrodynamics, X-rays, ultrasonics

    CERN Document Server

    Früngel, Frank B A

    1965-01-01

    High Speed Pulse Technology, Volume 1: Capacitor Discharges - Magnetohydrodynamics - X-Rays - Ultrasonics deals with the theoretical and engineering problems that arise in the capacitor discharge technique.This book discusses the characteristics of dielectric material, symmetrical switch tubes with mercury filling, and compensation conductor forms. The transformed discharge for highest current peaks, ignition transformer for internal combustion engines, and X-ray irradiation of subjects in mechanical motion are also elaborated. This text likewise covers the transformed capacitor discharge in w

  19. Supernova remnants: the X-ray perspective

    OpenAIRE

    Vink, Jacco

    2011-01-01

    Supernova remnants are beautiful astronomical objects that are also of high scientific interest, because they provide insights into supernova explosion mechanisms, and because they are the likely sources of Galactic cosmic rays. X-ray observations are an important means to study these objects.And in particular the advances made in X-ray imaging spectroscopy over the last two decades has greatly increased our knowledge about supernova remnants. It has made it possible to map the products of fr...

  20. Scattered X-ray beam nondestructive testing

    Science.gov (United States)

    Harding, G.; Kosanetzky, J.

    1989-08-01

    X-ray scatter interactions generally dominate the linear attenuation coefficient at the photon energies typical of medical and industrial radiography. Specific advantages of X-ray scatter imaging, including a flexible choice of measurement geometry, direct 3D-imaging capability (tomography) and improved information for material characterization, are illustrated with results from Compton and coherent scatter devices. Applications of a Compton backscatter scanner (ComScan) in the aerospace industry and coherent scatter imaging in security screening are briefly considered.