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Sample records for total reflection x-ray

  1. Total reflection X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Michaelis, W.; Prange, A.

    1987-01-01

    In the past few years, total reflection X-ray flourescence analysis (TXRF) has found an increasing number of assignments and applications. Experience of trace element analysis using TXRF and examples of applications are already widespread. Therefore, users of TXRF had the opportunity of an intensive exchange of their experience at the 1st workshop on total reflection X-ray fluorescence analysis which took place on May 27th and 28th 1986 at the GKSS Research Centre at Geesthacht. In a series of lectures and discussions dealing with the analytical principle itself, sample preparation techniques and applications as well as comuter programs for spectrum evaluation, the present state of development and the range of applications were outlined. 3 studies out of a total of 14 were included separately in the INIS and ENERGY databases. With 61 figs., 12 tabs [de

  2. Total reflection X-ray photoelectron spectroscopy: A review

    International Nuclear Information System (INIS)

    Kawai, Jun

    2010-01-01

    Total reflection X-ray photoelectron spectroscopy (TRXPS) is reviewed and all the published papers on TRXPS until the end of 2009 are included. Special emphasis is on the historical development. Applications are also described for each report. The background reduction is the most important effect of total reflection, but interference effect, relation to inelastic mean free path, change of probing depth are also discussed.

  3. Total-reflection x-ray fluorescence with a brillant undulator x-ray source

    International Nuclear Information System (INIS)

    Sakurai, K.; Eba, H.; Numako, C.; Suzuki, M.; Inoue, K.; Yagi, N.

    2000-01-01

    Total-reflection x-ray fluorescence (TXRF) is a highly sensitive technique for analyzing trace elements, because of the very low background from the sample support. Use of third-generation synchrotron x-ray source could further enhance the detection power. However, while such high sensitivity permits the detection of signals from trace elements of interest, it also means that one can observe weak parasitic x-rays as well. If the sample surface becomes even slightly contaminated, owing to air particulates near the beamline, x-ray fluorescence lines of iron, zinc, copper, nickel, chromium, and titanium can be observed even for a blank sample. Another critical problem is the low-energy-side tail of the scattering x-rays, which ultimately restricts the detection capability of the technique using a TXRF spectrometer based on a Si(Li) detector. The present paper describes our experiments with brilliant undulator x-ray beams at BL39XU and BL40XU, at the SPring-8, Harima, Japan. The emphasis is on the development of instruments to analyze a droplet of 0.1 μl containing trace elements of ppb level. Although the beamline is not a clean room, we have employed equipment for preparing a clean sample and also for avoiding contamination during transferring the sample into the spectrometer. We will report on the successful detection of the peak from 0.8 ppb selenium in a droplet (absolute amount 80 fg). We will also present the results of recent experiments obtained from a Johansson spectrometer rather than a Si(Li) detector. (author)

  4. Total reflection x-ray fluorescence - an approach to nanoanalysis

    International Nuclear Information System (INIS)

    Klockenkaemper, R.

    2000-01-01

    X-ray fluorescence analysis (XRFA) is a powerful tool used for industrial production, geological prospecting and for environmental control. However, the method suffers from a lack of sensitivity so that analyses are restricted to microanalytical investigations. That means: the sample amount needed for analysis is above some 10 micrograms, concentrations to be determined have to be on the μg/ml level, and thin layers to be characterized must be of micrometer thickness. In contrast to conventional XRFA, total-reflection X-ray fluorescence (TXRF) is extremely sensitive and even allows nano-analytical investigations. Three different ways can be taken: (i) use of minute sample amounts of only 10 nano-grams, (ii) determination of extreme traces below ng/ml and (iii) surface analysis and depth profiling of shallow layers with nano-meter thickness. In this lecture, the basic physical phenomena of total reflection and standing waves are outlined. The experimental equipment for TXRF is sketched out and commercially available instruments of different manufacturers are compared. Furthermore, examples are given for the three kinds of nano-analytical applications: ultra-micro, analysis, ultra trace analysis and mono- and thin-layer analysis. (author)

  5. Determination of technetium by total reflection x-ray fluorescence

    International Nuclear Information System (INIS)

    Bermudez, J.I.; Greaves, E.D.; Nemeth, P.

    2000-01-01

    We describe a technique using total reflection x-ray fluorescence (TXRF) for determination of Technetium produced by elution of chromatography generators with physiological saline solutions. The analysis with the 18.41 keV K α line of Technetium was accomplished with monochromatized K α radiation from a silver anode x-ray tube operated at 45 keV and 20 mA. This radiation at 22.104 keV is efficiently coupled to the 21.054 keV absorption edge of Tc. It is also of advantage in the direct analysis of organic and saline properties of the Tc-bearing samples. Quantification was accomplished by internal standard addition of Ga and using an interpolated value of the sensitivity for Tc between Molybdenum and Rhenium. Data processing was carried out with the QXAS-AXIL software package. System sensitivity was found adequate for direct Tc determination of eluted saline solutions. The interest and advantages of the use of the technique as an auxiliary in the synthesis and characterization of Tc-labeled radiopharmaceuticals used for diagnosis in nuclear medicine are discussed. Detection limits in the matrices analyzed are reported. (author)

  6. Application of total reflection X-ray fluorescence spectrometry for ...

    Indian Academy of Sciences (India)

    Applicability of total reflection X-ray fluorescence (TXRF) spectrometry for trace elemental analysis of rainwater samples was studied. The study was used to develop these samples as rainwater standards by the National University of Singapore (NUS). Our laboratory was one of the participants to use TXRF for this study.

  7. Determination of sulphur with total reflection x-ray spectrometry

    International Nuclear Information System (INIS)

    Steinmeyer, S.; Kolbesen, B.O.

    2000-01-01

    The potential and limitations of total reflection x-ray spectrometry (TXRF) were tested for the quantitative determination of the light element sulphur in inorganic and biological samples. As representatives of inorganic samples alkali, transition metal, magnesium and aluminum sulphates were investigated. As biological samples the sulphur containing amino acid methionine and the pharmaceutical drug insulin were chosen. All measurements were performed on a TXRF-spectrometer EXTRA IIA (Atomika Instruments, Oberschleissheim/Germany) using tungsten L-radiation as the excitation tube. Various concentrations of all samples ranging from 20 mg/l to 0.5 mg/l were determined. In addition the surface topography and thickness of the dry residue of these samples were investigated with SEM and a thickness profilometer (Alpha-Step). The result show that the reliable determination of sulphur in sulphates depends on the cation involved. Alkali sulphates like Na 2 SO 4 , or K 2 SO 4 form bulky residues resulting in significant deviations of the recovery rate of sulphur. In this case the use of smoothing detergents like 1 % HF, 1 % malic acid and 2 % hydrazinhydrat was found to be necessary for accurate determination. The results for the biological samples agree well with the expected values. The investigations lead to the conclusion that TXRF combined with a proper samples preparation is well suited for the determination of sulphur in different samples with various concentrations and matrices. (author)

  8. Thin film characterization by total reflection x-ray fluorescence

    International Nuclear Information System (INIS)

    Danel, Adrien; Nolot, Emmanuel; Veillerot, Marc; Olivier, Segolene; Decorps, Tifenn; Calvo-Munoz, Maria-Luisa; Hartmann, Jean-Michel; Lhostis, Sandrine; Kohno, Hiroshi; Yamagami, Motoyuki; Geoffroy, Charles

    2008-01-01

    Sensitive and accurate characterization of films thinner than a few nm used in nanoelectronics represents a challenge for many conventional production metrology tools. With capabilities in the 10 10 at/cm 2 , methods usually dedicated to contamination analysis appear promising, especially Total-reflection X-Ray Fluorescence (TXRF). This study shows that under usual configuration for contamination analysis, with incident angle smaller than the critical angle of the substrate, TXRF signal saturation occurs very rapidly for dense films (below 0.5 nm for HfO 2 films on Si wafers using a 9.67 keV excitation at 0.5 deg.). Increasing the incident angle, the range of linear results can be extended, but on the other hand, the TXRF sensitivity is degraded because of a strong increase of the measurement dead time. On HfO 2 films grown on Si wafers, an incident angle of 0.32 deg. corresponding to a dead time of 95% was used to achieve linear analysis up to 2 nm. Composition analysis by TXRF, and especially the detection of minor elements into thin films, requires the use of a specific incident angle to optimize sensitivity. Although quantitative analyses might require specific calibration, this work shows on Co-based films that the ratio between minor elements (W, P, Mo) and Co taking into account their relative sensitivity factors is a good direct reading of the composition

  9. X-ray total reflection mirrors for coherent illumination

    CERN Document Server

    Ishikawa, T; Yabashi, M; Souvorov, A; Yamauchi, K; Yamamura, K; Mimura, H; Saito, A; Mori, Y

    2002-01-01

    X-ray mirrors for coherent illumination demand much higher surface quality than is achievable with the conventional polishing techniques. Plasma chemical vaporization machining (CVM) and elastic emission machining (EEM) have been applied for x-ray mirror manufacturing. Figure error of a flat silicon single crystal mirrors made with CVM+EEM process was reduced to 2.0 nm peak-to-valley and 0.2 nm RMS. The machining process was also applied to make elliptical mirrors. One-dimensional focusing with a single elliptical mirror showed diffraction-limited properties with the focal width of 200 nm. Two-dimensional focusing with Kirkpatric-Baez configuration gave a focal spot size of 200 nm x 200 nm. (author)

  10. Sweeping total reflection X-ray fluorescence optimisation to monitor the metallic contamination into IC manufacturing

    International Nuclear Information System (INIS)

    Borde, Yannick; Danel, Adrien; Roche, Agnes; Veillerot, Marc

    2008-01-01

    Among the methods available on the market today to control as metallic contamination in integrated circuit manufacturing, Sweeping Total reflection X-ray Fluorescence mode appears a very good method, providing fast and entire wafer mapping. With the goal of a pertinent use of Sweeping Total reflection X-ray Fluorescence in advanced Integrated Circuit manufacturing this work discusses how acceptable levels of contamination specified by the production (low levels to be detected) can be taken into account. The relation between measurement results (surface coverage, throughput, low limit of detection, limit of quantification, quantification of localized contamination) and Sweeping Total reflection X-ray Fluorescence parameters (number of measurement points and integration time per point) is presented in details. In particular, a model is proposed to explain the mismatch between actual surface contamination in a localized spot on wafer and Total reflection X-ray Fluorescence reading. Both calibration and geometric issues have been taken into account

  11. Forensic application of total reflection X-ray fluorescence spectrometry for elemental characterization of ink samples

    International Nuclear Information System (INIS)

    Dhara, Sangita; Misra, N.L.; Maind, S.D.; Kumar, Sanjukta A.; Chattopadhyay, N.; Aggarwal, S.K.

    2010-01-01

    The possibility of applying Total Reflection X-ray Fluorescence for qualitative and quantitative differentiation of documents printed with rare earth tagged and untagged inks has been explored in this paper. For qualitative differentiation, a very small amount of ink was loosened from the printed documents by smoothly rubbing with a new clean blade without destroying the manuscript. 50 μL of Milli-Q water was put on this loose powder, on the manuscript, and was agitated by sucking and releasing the suspension two to three times with the help of a micropipette. The resultant dispersion was deposited on quartz sample support for Total Reflection X-ray Fluorescence measurements. The Total Reflection X-ray Fluorescence spectrum of tagged and untagged inks could be clearly differentiated. In order to see the applicability of Total Reflection X-ray Fluorescence for quantitative determinations of rare earths and also to countercheck such determinations in ink samples, the amounts of rare earth in painted papers with single rare earth tagged inks were determined by digesting the painted paper in HNO 3 /HClO 4 , mixing this solution with the internal standard and recording their Total Reflection X-ray Fluorescence spectra after calibration of the instrument. The results thus obtained were compared with those obtained by Inductively Coupled Plasma Mass Spectrometry and were found in good agreement. The average precision of the Total Reflection X-ray Fluorescence determinations was 5.5% (1σ) and the average deviation of Total Reflection X-ray Fluorescence determined values with that of Inductively Coupled Plasma Mass Spectrometry was 7.3%. These studies have shown that Total Reflection X-ray Fluorescence offers a promising and potential application in forensic work of this nature.

  12. Forensic application of total reflection X-ray fluorescence spectrometry for elemental characterization of ink samples

    Energy Technology Data Exchange (ETDEWEB)

    Dhara, Sangita [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Misra, N.L., E-mail: nlmisra@barc.gov.i [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Maind, S.D. [NAA Unit of Central Forensic Science Laboratory Hyderabad at Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Kumar, Sanjukta A. [Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Chattopadhyay, N. [NAA Unit of Central Forensic Science Laboratory Hyderabad at Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Aggarwal, S.K. [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India)

    2010-02-15

    The possibility of applying Total Reflection X-ray Fluorescence for qualitative and quantitative differentiation of documents printed with rare earth tagged and untagged inks has been explored in this paper. For qualitative differentiation, a very small amount of ink was loosened from the printed documents by smoothly rubbing with a new clean blade without destroying the manuscript. 50 muL of Milli-Q water was put on this loose powder, on the manuscript, and was agitated by sucking and releasing the suspension two to three times with the help of a micropipette. The resultant dispersion was deposited on quartz sample support for Total Reflection X-ray Fluorescence measurements. The Total Reflection X-ray Fluorescence spectrum of tagged and untagged inks could be clearly differentiated. In order to see the applicability of Total Reflection X-ray Fluorescence for quantitative determinations of rare earths and also to countercheck such determinations in ink samples, the amounts of rare earth in painted papers with single rare earth tagged inks were determined by digesting the painted paper in HNO{sub 3}/HClO{sub 4}, mixing this solution with the internal standard and recording their Total Reflection X-ray Fluorescence spectra after calibration of the instrument. The results thus obtained were compared with those obtained by Inductively Coupled Plasma Mass Spectrometry and were found in good agreement. The average precision of the Total Reflection X-ray Fluorescence determinations was 5.5% (1sigma) and the average deviation of Total Reflection X-ray Fluorescence determined values with that of Inductively Coupled Plasma Mass Spectrometry was 7.3%. These studies have shown that Total Reflection X-ray Fluorescence offers a promising and potential application in forensic work of this nature.

  13. Total-reflection X-ray fluorescence analysis of Austrian wine

    Energy Technology Data Exchange (ETDEWEB)

    Gruber, X. [Atominstitut der Osterreichischen Universitaeten, 1020 Vienna (Austria); Kregsamer, P. [Atominstitut der Osterreichischen Universitaeten, 1020 Vienna (Austria); Wobrauschek, P. [Atominstitut der Osterreichischen Universitaeten, 1020 Vienna (Austria); Streli, C. [Atominstitut der Osterreichischen Universitaeten, 1020 Vienna (Austria)]. E-mail: streli@ati.ac.at

    2006-11-15

    The concentration of major, minor and trace elements in Austrian wine was determined by total-reflection X-ray fluorescence using gallium as internal standard. A multi-elemental analysis was possible by pipetting 6 {mu}l of wine directly on the reflector and drying. Total-reflection X-ray fluorescence analysis was performed with Atomika EXTRA II A (Cameca) X-rays from a Mo tube with a high-energy cut-off at 20 keV in total-reflection geometry. The results showed that it was possible to identify only by the elemental analysis as fingerprint the vineyards and year of vintage among 11 different wines.

  14. Analysis of archaeological ceramics by total-reflection X-ray fluorescence: Quantitative approaches

    International Nuclear Information System (INIS)

    Fernandez-Ruiz, R.; Garcia-Heras, M.

    2008-01-01

    This paper reports the quantitative methodologies developed for the compositional characterization of archaeological ceramics by total-reflection X-ray fluorescence at two levels. A first quantitative level which comprises an acid leaching procedure, and a second selective level, which seeks to increase the number of detectable elements by eliminating the iron present in the acid leaching procedure. Total-reflection X-ray fluorescence spectrometry has been compared, at a quantitative level, with Instrumental Neutron Activation Analysis in order to test its applicability to the study of this kind of materials. The combination of a solid chemical homogenization procedure previously reported with the quantitative methodologies here presented allows the total-reflection X-ray fluorescence to analyze 29 elements with acceptable analytical recoveries and accuracies

  15. Total-reflection X-ray fluorescence analysis of Austrian wine

    International Nuclear Information System (INIS)

    Gruber, X.; Kregsamer, P.; Wobrauschek, P.; Streli, C.

    2006-01-01

    The concentration of major, minor and trace elements in Austrian wine was determined by total-reflection X-ray fluorescence using gallium as internal standard. A multi-elemental analysis was possible by pipetting 6 μl of wine directly on the reflector and drying. Total-reflection X-ray fluorescence analysis was performed with Atomika EXTRA II A (Cameca) X-rays from a Mo tube with a high-energy cut-off at 20 keV in total-reflection geometry. The results showed that it was possible to identify only by the elemental analysis as fingerprint the vineyards and year of vintage among 11 different wines

  16. Analysis of archaeological ceramics by total-reflection X-ray fluorescence: Quantitative approaches

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Servicio Interdepartamental de Investigacion, Facultad de Ciencias, Universidad Autonoma de Madrid, Modulo C-9, Laboratorio de TXRF, Crta. Colmenar, Km 15, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Garcia-Heras, M. [Grupo de Arqueometria de Vidrios y Materiales Ceramicos, Instituto de Historia, Centro de Ciencias Humanas y Sociales, CSIC, C/ Albasanz, 26-28, 28037 Madrid (Spain)

    2008-09-15

    This paper reports the quantitative methodologies developed for the compositional characterization of archaeological ceramics by total-reflection X-ray fluorescence at two levels. A first quantitative level which comprises an acid leaching procedure, and a second selective level, which seeks to increase the number of detectable elements by eliminating the iron present in the acid leaching procedure. Total-reflection X-ray fluorescence spectrometry has been compared, at a quantitative level, with Instrumental Neutron Activation Analysis in order to test its applicability to the study of this kind of materials. The combination of a solid chemical homogenization procedure previously reported with the quantitative methodologies here presented allows the total-reflection X-ray fluorescence to analyze 29 elements with acceptable analytical recoveries and accuracies.

  17. Surface characterization of selected polymer thin films by total-reflection x-ray fluorescence spectroscopy and x-ray reflectivity

    International Nuclear Information System (INIS)

    Innis, Vallerie Ann A.

    2006-01-01

    Development of available x-ray characterizations tools for grazing incidence techniques was done to be able to probe nano-size thin films. Alignment of a Philips x-ray powder diffractometer was improved to let it perform as an x-ray reflectometer. X-ray reflectometry was coupled with total-reflection x-ray fluorescence spectroscopy. Evaluation of the performance of this grazing incidence techniques was done by preparing polymer thin films of carboxymethylcellulose, carrageenan and polyvinylpyrrolidone (PVP). The thickness of the films were varied by varying the process parameters such as concentration, spin speed and spin time. Angle-dispersive total-reflection x-ray fluorescence spectroscopy profiles of three films showed film formation only in carrageenan and PVP. For both carrageenan and PVP, an increase in concentration yielded a corresponding increase in intensity of the fluorescent or scattered peaks. XRR profiles of carrageenan thin films yielded a mean value for the critical angle close to quartz substrate. Thickness measurements of the prepared carrageenan thin films showed that concentration was the main determinant for final film thickness over the other process parameters. Sulfur fluorescent intensity derived from the TXRF measurement showed a linear relationship with the measured thickness by XRR. For PVP, measured critical angle is lower than quartz. Poor adhesion of the polymer onto the substrate yielded a limited number of thickness measurements made from the XRR profiles. (Author)

  18. Development of a total reflection X-ray fluorescence spectrometer for ...

    Indian Academy of Sciences (India)

    Unknown

    design and use of a peltier cooled solid state detector for energy dispersive detection. Alignment and ... X-ray beam at a glancing angle less than the critical angle at which total ... materials is < 1 so that external total reflection takes place at an ...

  19. Total and available metal contents in sediments by synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Moreira, Silvana; Sobrinho, Gilmar A.; Jesus, Edgar F.O. de; Lopes, Ricardo T.

    2002-01-01

    In this work the total and available contents of Al, Si, Cl, K, Mn, Fe, Co, Ni, Cu, Zn, Sr, Zr, Ba, Ce and Pb in sediments from river Atibaia were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence technique. The detection limits for K series varies from 200 ng.mL -1 for Al to 2 ng.mL -1 for Zn while for L series the value varies from 20 ng.mL -1 for Ba to 10 ng.mL -1 for Pb. The samples were submitted to two different processes, in order to obtain the total and biological available metal contents. The information about metal content is a important parameter for a correct evaluation about the hydrologic cycle in Piracicaba basin. All the measure were carried out at the National Synchrotron Light Laboratory, Campinas, SP, Brazil, using a white beam for excitation. (author)

  20. Microanalysis of old violin varnishes by total-reflection X-ray fluorescence

    Science.gov (United States)

    von Bohlen, Alex; Meyer, Friedrich

    1997-07-01

    Total reflection X-ray fluorescence was used to characterize elements (with Z>13) contained in varnishes applied by prominent violin makers during the last five centuries. Direct analyses of small flakes with masses varnish. Higher amounts of Fe, As and Pb were found in old products, Mn, Co, Cu, Zn and Pb were used in more recent varnishes.

  1. Total reflection X-ray fluorescence with synchrotron radiation applied to biological and environmental samples

    International Nuclear Information System (INIS)

    Simabuco, S.M.; Matsumoto, E.; Jesus, E.F.O.; Lopes, R.T.; Perez, C.; Nascimento Filho, V.F.; Costa, R.S.S.; Tavares do Carmo, M.G.; Saunders, C.

    2001-01-01

    Full text: The Total Reflection X-ray Fluorescence has been applied for trace elements in water and aqueous solutions, environmental samples and biological materials after sample preparation and to surface analysis of silicon wafers. The present paper shows some results of applications for rainwater, atmospheric particulate material, colostrum and nuclear samples. (author)

  2. Characterization of atmospheric aerosols using Synchroton radiation total reflection X-ray fluorescence and Fe K-edge total reflection X-ray fluorescence-X-ray absorption near-edge structure

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, U.E.A. [Department of Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany)], E-mail: ursula.fittschen@chemie.uni-hamburg.de; Meirer, F. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria)], E-mail: fmeirer@ati.ac.at; Streli, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria)], E-mail: streli@ati.ac.at; Wobrauschek, P. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria)], E-mail: wobi@ati.ac.at; Thiele, J. [Department of Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany)], E-mail: Julian.Thiele@gmx.de; Falkenberg, G. [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22603 Hamburg (Germany)], E-mail: falkenbe@mail.desy.de; Pepponi, G. [ITC-irst, Via Sommarive 18, 38050 Povo (Trento) (Italy)], E-mail: pepponi@itc.it

    2008-12-15

    In this study a new procedure using Synchrotron total reflection X-ray fluorescence (SR-TXRF) to characterize elemental amounts in atmospheric aerosols down to particle sizes of 0.015 um is presented. The procedure was thoroughly evaluated regarding bounce off effects and blank values. Additionally the potential of total reflection X-ray fluorescence-X-ray absorption near edge structure (SR-TXRF-XANES) for speciation of FeII/III down to amounts of 34 pg in aerosols which were collected for 1 h is shown. The aerosols were collected in the city of Hamburg with a low pressure Berner impactor on Si carriers covered with silicone over time periods of 60 and 20 min each. The particles were collected in four and ten size fractions of 10.0-8.0 {mu}m, 8.0-2.0 {mu}m, 2.0-0.13 {mu}m 0.13-0.015 {mu}m (aerodynamic particle size) and 15-30 nm, 30-60 nm, 60-130 nm, 130-250 nm, 250-500 nm, 0.5-1 {mu}m, 1-2 {mu}m, 2-4 {mu}m, 4-8 {mu}m, 8-16 {mu}m. Prior to the sampling 'bounce off' effects on Silicone and Vaseline coated Si carriers were studied with total reflection X-ray fluorescence. According to the results silicone coated carriers were chosen for the analysis. Additionally, blank levels originating from the sampling device and the calibration procedure were studied. Blank levels of Fe corresponded to 1-10% of Fe in the aerosol samples. Blank levels stemming from the internal standard were found to be negligible. The results from the Synchroton radiation total reflection X-ray fluorescence analysis of the aerosols showed that 20 min of sampling time gave still enough sample material for elemental determination of most elements. For the determination of the oxidation state of Fe in the aerosols different Fe salts were prepared as a reference from suspensions in isopropanol. The results from the Fe K-edge Synchroton radiation total reflection X-ray fluorescence-X-ray absorption near-edge structure analysis of the aerosol samples showed that mainly Fe(III) was present in

  3. Characterization of atmospheric aerosols using Synchroton radiation total reflection X-ray fluorescence and Fe K-edge total reflection X-ray fluorescence-X-ray absorption near-edge structure

    International Nuclear Information System (INIS)

    Fittschen, U.E.A.; Meirer, F.; Streli, C.; Wobrauschek, P.; Thiele, J.; Falkenberg, G.; Pepponi, G.

    2008-01-01

    In this study a new procedure using Synchrotron total reflection X-ray fluorescence (SR-TXRF) to characterize elemental amounts in atmospheric aerosols down to particle sizes of 0.015 um is presented. The procedure was thoroughly evaluated regarding bounce off effects and blank values. Additionally the potential of total reflection X-ray fluorescence-X-ray absorption near edge structure (SR-TXRF-XANES) for speciation of FeII/III down to amounts of 34 pg in aerosols which were collected for 1 h is shown. The aerosols were collected in the city of Hamburg with a low pressure Berner impactor on Si carriers covered with silicone over time periods of 60 and 20 min each. The particles were collected in four and ten size fractions of 10.0-8.0 μm, 8.0-2.0 μm, 2.0-0.13 μm 0.13-0.015 μm (aerodynamic particle size) and 15-30 nm, 30-60 nm, 60-130 nm, 130-250 nm, 250-500 nm, 0.5-1 μm, 1-2 μm, 2-4 μm, 4-8 μm, 8-16 μm. Prior to the sampling 'bounce off' effects on Silicone and Vaseline coated Si carriers were studied with total reflection X-ray fluorescence. According to the results silicone coated carriers were chosen for the analysis. Additionally, blank levels originating from the sampling device and the calibration procedure were studied. Blank levels of Fe corresponded to 1-10% of Fe in the aerosol samples. Blank levels stemming from the internal standard were found to be negligible. The results from the Synchroton radiation total reflection X-ray fluorescence analysis of the aerosols showed that 20 min of sampling time gave still enough sample material for elemental determination of most elements. For the determination of the oxidation state of Fe in the aerosols different Fe salts were prepared as a reference from suspensions in isopropanol. The results from the Fe K-edge Synchroton radiation total reflection X-ray fluorescence-X-ray absorption near-edge structure analysis of the aerosol samples showed that mainly Fe(III) was present in all particle size fractions

  4. An optimised set-up for total reflection particle induced X-ray emission

    International Nuclear Information System (INIS)

    Kan, J.A. van; Vis, R.D.

    1997-01-01

    MeV proton beams at small angles of incidence (0-35 mrad) are used to analyse trace elements on flat surfaces such as Si wafers or quartz substrates. In these experiments, the particle induced X-ray emission (PIXE) signal is used in a new optimized set-up. This set-up is constructed in such a way that the X-ray detector can reach very large solid angles, larger than 1 sr. Use of these large detector solid angles, combined with the reduction of bremsstrahlung background, affords limits of detection (LOD) of the order of 10 10 at cm -2 using total reflection particle induced X-ray emission (TPIXE). The LODs from earlier TPIXE measurements in a non-optimized set-up are used to estimate LODs in the new TPIXE set-up. Si wafers with low surface concentrations of V, Ni, Cu and Ag are used as standards to calibrate the LODs found with this set-up. The metal concentrations are determined by total reflection X-ray fluorescence (TXRF). The TPIXE measurements are compared with TXRF measurements on the same wafers. (Author)

  5. Confocal total reflection X-ray fluorescence technology based on an elliptical monocapillary and a parallel polycapillary X-ray optics.

    Science.gov (United States)

    Zhu, Yu; Wang, Yabing; Sun, Tianxi; Sun, Xuepeng; Zhang, Xiaoyun; Liu, Zhiguo; Li, Yufei; Zhang, Fengshou

    2018-07-01

    A total reflection X-ray fluorescence (TXRF) spectrometer based on an elliptical monocapillary X-ray lens (MXRL) and a parallel polycapillary X-ray lens (PPXRL) was designed. This TXRF instrument has micro focal spot, low divergence and high intensity of incident X-ray beam. The diameter of the focal spot of MXRL was 16.5 µm, and the divergence of the incident X-ray beam was 3.4 mrad. We applied this TXRF instrument to the micro analysis of a single-layer film containing Ni deposited on a Si substrate by metal vapor vacuum arc ion source. Copyright © 2018 Elsevier Ltd. All rights reserved.

  6. Abstracts of the 8th Conference on total reflection x-ray fluorescence analysis and related methods

    International Nuclear Information System (INIS)

    Wobrauschek, P.

    2000-01-01

    The 8. conference on total reflection x-ray fluorescence analysis and related methods held from 25.9 to 29.9.2000 contains 79 abstracts about x-ray fluorescence analysis (XRFA) as a powerful tool used for industrial production, geological prospecting and for environmental control. Total reflection x-ray fluorescence spectroscopy is also a tool used for chemical analysis in medicine, industry and research. (E.B.)

  7. Application of the Total Reflection X-ray Fluorescence technique to trace elements determination in tobacco

    International Nuclear Information System (INIS)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2008-01-01

    Many studies have identified an important number of toxic elements along with organic carcinogen molecules and radioactive isotopes in tobacco. In this work we have analyzed by Total Reflection X-Ray Fluorescence 9 brands of cigarettes being manufactured and distributed in the Mexican market. Two National Institute of Standards and Technology standards and a blank were equally treated at the same time. Results show the presence of some toxic elements such as Pb and Ni. These results are compared with available data for some foreign brands, while their implications for health are discussed. It can be confirmed that the Total Reflection X-Ray Fluorescence method provides precise (reproducible) and accuracy (trueness) data for 15 elements concentration in tobacco samples

  8. Application of the Total Reflection X-ray Fluorescence technique to trace elements determination in tobacco

    Science.gov (United States)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2008-12-01

    Many studies have identified an important number of toxic elements along with organic carcinogen molecules and radioactive isotopes in tobacco. In this work we have analyzed by Total Reflection X-Ray Fluorescence 9 brands of cigarettes being manufactured and distributed in the Mexican market. Two National Institute of Standards and Technology standards and a blank were equally treated at the same time. Results show the presence of some toxic elements such as Pb and Ni. These results are compared with available data for some foreign brands, while their implications for health are discussed. It can be confirmed that the Total Reflection X-Ray Fluorescence method provides precise (reproducible) and accuracy (trueness) data for 15 elements concentration in tobacco samples.

  9. Applications of total reflection X-ray fluorescence in multi-element analysis

    International Nuclear Information System (INIS)

    Michaelis, W.; Prange, A.; Knoth, J.

    1985-01-01

    Although Total Reflection X-Ray Fluorescence Analysis (TXRF) became available for practical applications and routine measurements only few years ago, the number of programmes that make use of this method is increasing rapidly. The scope of work is widespread over environmental research and monitoring, mineralogy, mineral exploration, oceanography, biology, medicine and biochemistry. The present paper gives a brief survey of these applications and summarizes some of them which are typical for quite different matrices. (orig.)

  10. Synchrotron radiation total reflection X-ray fluorescence (SR-TXRF) for evaluation of food contamination

    International Nuclear Information System (INIS)

    Vives, A.E.S.; Brienza, S.M.B.; Moreira, S.; Zucchi, O.L.A.; Nascimento Filho, V.F.

    2006-01-01

    The objective of this study was to use synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF) for the determination of metals and other elements in food available to the population in commercial establishments, in order to evaluate the risks of contamination by these products. The analyzed species were vegetables, leafy vegetables, fruits, cereal and grain. The results indicated that some species were contaminated by Cr, Cu, Zn and Pb with concentrations much higher than the reference values. (author)

  11. Total reflection X-ray fluorescence analysis with synchrotron radiation monochromatized by multilayer structures

    International Nuclear Information System (INIS)

    Rieder, R.; Wobrauschek, P.; Ladisich, W.; Streli, C.; Aiginger, H.; Garbe, S.; Gaul, G.; Knoechel, A.; Lechtenberg, F.

    1995-01-01

    To achieve lowest detection limits in total reflection X-ray fluorescence analysis (TXRF) synchrotron radiation has been monochromatized by a multilayer structure to obtain a relative broad energy band compared to Bragg single crystals for an efficient excitation. The energy has been set to 14 keV, 17.5 keV, 31 keV and about 55 keV. Detection limits of 20 fg and 150 fg have been achieved for Sr and Cd, respectively. ((orig.))

  12. Total Reflection X-ray Fluorescence Analysis (TXRF) using the high flux SAXS camera

    CERN Document Server

    Wobrauschek, P; Pepponi, G; Bergmann, A; Glatter, O

    2002-01-01

    Combining the high photon flux from a rotating anode X-ray tube with an X-ray optical component to focus and monochromatize the X-ray beam is the most promising instrumentation for best detection limits in the modern XRF laboratory. This is realized by using the design of a high flux SAXS camera in combination with a 4 kW high brilliant rotating Cu anode X-ray tube with a graded elliptically bent multilayer and including a new designed module for excitation in total reflection geometry within the beam path. The system can be evacuated thus reducing absorption and scattering of air and removing the argon peak in the spectra. Another novelty is the use of a Peltier cooled drift detector with an energy resolution of 148 eV at 5.9 keV and 5 mm sup 2 area. For Co detection limits of about 300 fg determined by a single element standard have been achieved. Testing a real sample NIST 1643d led to detection limits in the range of 300 ng/l for the medium Z.

  13. TX 2000: total reflection and 45o energy dispersive x-ray fluorescence spectrometer

    International Nuclear Information System (INIS)

    Pasti, F.; Torboli, A.; Valdes, M.

    2000-01-01

    This equipment, developed by Ital Structures, combines two kinds of energy dispersive X-ray fluorescence techniques, the first using total reflection geometry and the second conventional 45 o geometry. The equipment is completely controlled by a PC and to reach the condition of total reflection is very easy because it is enough to load the file with the right position for the corresponding energy. In this apparatus we used an x-ray tube with an alloy anode of Mo/W with a long fine focus at 2200 W. To monochromatize the x-ray beam while choosing, for example, the Mo K alpha or W L alpha or a piece of white spectrum of 33 keV, we use a highly reflective multilayer made of Si/W with 2d = 45.5 A o . The detector used in the equipment is a lithium drifted silicon detector (Si(Li)) with an excellent energy resolution of 135 eV at 5.9 keV and 1000 cps. We developed two programs written in Windows 95, 98 and NT for a 32 bit microprocessor. The first one is called TYACQ32 and has the following functions: first, complete control of the hardware, second automatic alignment of the TX 2000 spectrometer and third acquisition of spectra. The second program is EDXRF32. This is a program to accomplish spectrum and quantitative analysis for TXRF and EDXRF 45 o degrees analysis. (author)

  14. Trace elements determination in red and white wines using total-reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Anjos, M.J.; Lopes, R.T.; Jesus, E.F.O. de; Moreira, S.; Barroso, R.C.; Castro, C.R.F.

    2003-01-01

    Several wines produced in different regions from south of Brazil and available in markets in Rio de Janeiro were analyzed for their contents of elements such as: P, S, Cl, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb and Sr. Multi-element analysis was possible with simple sample preparation and subsequent analysis by total-reflection X-ray fluorescence using synchrotron radiation. The measurement was carried at the X-ray fluorescence beamline in the Synchrotron Light Source Laboratory in Campinas, Brazil. The levels of the various elements obtained were lower in the Brazilian wines than the values generally found in the literature. The present study indicates the capability of multi-element analysis for determining the contents of various elements present in wines coming from Brazil vineyards by using a simple, sensitive and precise method

  15. Single particle transfer for quantitative analysis with total-reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Esaka, Fumitaka; Esaka, Konomi T.; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu; Watanabe, Kazuo

    2006-01-01

    The technique of single particle transfer was applied to quantitative analysis with total-reflection X-ray fluorescence (TXRF) spectrometry. The technique was evaluated by performing quantitative analysis of individual Cu particles with diameters between 3.9 and 13.2 μm. The direct quantitative analysis of the Cu particle transferred onto a Si carrier gave a discrepancy between measured and calculated Cu amounts due to the absorption effects of incident and fluorescent X-rays within the particle. By the correction for the absorption effects, the Cu amounts in individual particles could be determined with the deviation within 10.5%. When the Cu particles were dissolved with HNO 3 solution prior to the TXRF analysis, the deviation was improved to be within 3.8%. In this case, no correction for the absorption effects was needed for quantification

  16. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    International Nuclear Information System (INIS)

    Moreira, Silvana; Vives, Ana Elisa S. de; Nascimento Filho, Virgilio F.; Zucchi, Orgheda L.D.A.

    2005-01-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 μL of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1μg.L -1 for Mn and Fe to 15μg.L -1 for P. (author)

  17. Beer analysis by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br; Zucchi, Orgheda L.D.A. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas de Ribeirao Preto]. E-mail: olzucchi@fcfrp.usp.br

    2005-07-01

    In this work the concentrations of P, S, Cl, K, Ca, Mn, Fe, Zn and Br in twenty-nine brands of national and international beers were determined by Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF). The results were compared with the limits established by the Brazilian Legislation and the nutritive values established by National Agricultural Library (NAL). The measurements were performed at the X-ray Fluorescence Beamline at Synchrotron Light Source Laboratory, in Campinas, Sao Paulo, Brazil, using a polychromatic beam for excitation. A small volume of 5 {mu}L of sample beers containing just an internal standard, used to correct geometry effects, were analyzed without any pre-treatment. The measuring time was 100 s and the detection limits obtained varied from 1{mu}g.L{sup -1} for Mn and Fe to 15{mu}g.L{sup -1} for P. (author)

  18. Total reflection X-ray Fluorescence determination of interfering elements rubidium and uranium by profile fitting

    Science.gov (United States)

    Dhara, Sangita; Khooha, Ajay; Singh, Ajit Kumar; Tiwari, M. K.; Misra, N. L.

    2018-06-01

    Systematic studies to assess the analytical parameters obtained in the total reflection X-ray fluorescence (TXRF) determinations of interfering elements Rb and U using profile fitting are reported in the present manuscript. The X-ray lines Rb Kα and U Lα having serious spectral interference (ΔE = 218 eV), have been used as analytical lines. The intensities of these X-ray lines have been assessed using profile fitting. In order to compare the analytical results of Rb determinations in presence of U, with and without U excitation, synchrotron radiation was tuned to energy just above and below the U Labs edge. This approach shall excite both Rb Kα and U Lα simultaneously and Rb Kα selectively. Finally, the samples were also analyzed with a laboratory based TXRF spectrometer. The analytical results obtained in all these conditions were comparable. The authenticity of the results was assessed by analyzing U with respect to Rb in Rb2U(SO4)3, a standard reference material for U. The average precision obtained for TXRF determinations was below 3% (RSD, n = 3, 1σ) and the percent deviation of TXRF values from the expected values calculated on the basis of sample preparation was within 3%.

  19. The capabilities of total reflection X-ray fluorescence in the polymeric analytical field

    International Nuclear Information System (INIS)

    Vazquez, Cristina

    2004-01-01

    This paper presents the capabilities of total reflection X-ray fluorescence (TXRF) as analytical technique specially focused in high-viscosity polymer dispersions. Appropriate sample preparation procedures are described taking into account the time stability of these dispersions. Special remarks considering different ways for drying samples in order to obtain the most uniform deposited film are investigated focusing on the behavior of aqueous and viscous systems. Due to the difficulty found for obtaining a homogeneous mixture between sample and internal standard in such systems, the use of Compton incoherent scattering is discussed as an alternative procedure for trace quantification in high viscous systems without any mixing processes

  20. The capabilities of total reflection X-ray fluorescence in the polymeric analytical field*1

    Science.gov (United States)

    Vázquez, Cristina

    2004-08-01

    This paper presents the capabilities of total reflection X-ray fluorescence (TXRF) as analytical technique specially focused in high-viscosity polymer dispersions. Appropriate sample preparation procedures are described taking into account the time stability of these dispersions. Special remarks considering different ways for drying samples in order to obtain the most uniform deposited film are investigated focusing on the behavior of aqueous and viscous systems. Due to the difficulty found for obtaining a homogeneous mixture between sample and internal standard in such systems, the use of Compton incoherent scattering is discussed as an alternative procedure for trace quantification in high viscous systems without any mixing processes.

  1. Determination of heavy metals in Damascus drinking water using total reflection x-ray fluorescence

    International Nuclear Information System (INIS)

    Bakraji, E. H.; Karajo, J.

    2000-01-01

    Total reflection x-ray fluorescence spectrometry and chemical preconcentration have applied for multi-elemental analysis of Damascus drinking water. Water was taken directly from taps of several city sectors and analyzed for the following trace elements: Ti, V, Cr, Fe, Co, Ni, Cu, Zn, Se and Pb. The detection limits were found to be in the range of 0.1 to 0.4 μg/l. The mean levels of trace elements in the Damascus drinking water were below the World Health Organization drinking water quality guidelines. (author)

  2. Synchrotron total reflection X-ray fluorescence at BL-16 microfocus beamline of Indus-2

    Energy Technology Data Exchange (ETDEWEB)

    Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in; Singh, A. K., E-mail: mktiwari@rrcat.gov.in; Das, Gangadhar, E-mail: mktiwari@rrcat.gov.in; Chowdhury, Anupam, E-mail: mktiwari@rrcat.gov.in; Lodha, G. S., E-mail: mktiwari@rrcat.gov.in [Indus Synchrotrons Utilisation Division, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India)

    2014-04-24

    Determination of ultra trace elements is important in many disciplines both in basic and applied sciences. Numerous applications show their importance in medical science, environmental science, materials science, food processing and semiconductor industries and in maintaining the quality control of ultra pure chemicals and reagents. We report commissioning of a synchrotron based total reflection x-ray fluorescence (TXRF) facility on the BL-16 microfocus beamline of Indus-2. This paper describes the performance of the BL-16 TXRF spectrometer and the detailed description of its capabilities through examples of measured results.

  3. Total reflection X-ray fluorescence and archaeometry: Application in the Argentinean cultural heritage

    Energy Technology Data Exchange (ETDEWEB)

    Vazquez, Cristina [Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina); Laboratorio de Quimica de Sistemas Heterogeneos, Facultad de Ingenieria, Universidad de Buenos Aires, P. Colon 850 (C1063ACU), Buenos Aires (Argentina)], E-mail: Cristina.Vazquez@cnea.gov.ar; Albornoz, Ana [Agencia Rio Negro Cultura, Museo de la Patagonia F.P.Moreno, Centro Civico s/n Bariloche, Rio Negro (Argentina); Hajduk, Adam [CONICET, Museo de la Patagonia F.P.Moreno, Centro Civico s/n Bariloche, Rio Negro (Argentina); Elkin, Dolores [CONICET Instituto Nacional de Antropologia y Pensamiento Latinoamericano, 3 de febrero 1378 (C1426AEL) Buenos Aires (Argentina); Custo, Graciela; Obrustky, Alba [Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina)

    2008-12-15

    Archaeometry is an interdisciplinary research area involved in the development and use of scientific methods in order to answer questions concerned with the human history. In this way the knowledge of archaeological objects through advanced chemical and physical analyses permits a better preservation and conservation of the cultural heritage and also reveals materials and technologies used in the past. In this sense, analytical techniques play an important role in order to provide chemical information about cultural objects. Considering the non destructive characteristic of this study, analytical techniques must be adequate in order to prevent any alteration or damage and in addition to allow the conservation of their integrity. Taking into account the irreplaceable character of the archaeological and artistic materials considered in this study, analytical techniques must be adequate in order to prevent any alteration or damage and in addition to allow the conservation of their integrity. Total Reflection X-ray Fluorescence Spectrometry as a geometric variant of conventional X-ray fluorescence is a proved microanalytical technique considering the small amount of sample required for the analysis. A few micrograms are enough in order to reveal valuable information about elemental composition and in this context it is highly recommended for artwork studies. In this paper a case study is presented in which Total Reflection X-Ray Fluorescence Spectrometry has been successfully employed in the archaeometry field. Examples from Argentinean cultural heritage sites related with the determination of pigments in paintings on canvas and in rock sites as well as in underwater archaeology research are shown.

  4. Total Reflection X-ray Fluorescence attachment module modified for analysis in vacuum

    International Nuclear Information System (INIS)

    Wobrauschek, P.; Streli, C.; Kregsamer, P.; Meirer, F.; Jokubonis, C.; Markowicz, A.; Wegrzynek, D.; Chinea-Cano, E.

    2008-01-01

    Based on the design of the low cost Total Reflection X-Ray Fluorescence attachment module available since 1986 from Atominstitut (WOBRAUSCHEK-module) which can be attached to existing X-ray equipment, a new version was developed which allows the analysis of samples in vacuum. This design was in particular possible as the Peltier cooled light weight Silicon Drift Detector is following all adjustment procedures for total reflection as angle rotation and linear motion. The detector is mounted through a vacuum feed and O-ring tightening to the small vacuum chamber. The standard 30 mm round quartz, Si-wafer or Plexiglas reflectors are used to carry the samples. The reflectors are placed on the reference plane with the dried sample down looking facing in about 0.5 mm distance the up looking detector window. The reflectors are resting on 3 steel balls defining precisely the reference plane for the adjustment procedure. As the rotation axis of the module is in the plane of the reflector surface, angle dependent experiments can be made to distinguish between film and particulate type contamination of samples. Operating with a Mo anode at 50 kV and 40 mA with a closely attached multilayer monochromator and using a 10 mm 2 KETEK silicon drift detector with 8 μm Be window, a sensitivity of 70 cps/ng for Rb was measured and detection limits of 2 pg were obtained

  5. Direct analysis of biological samples by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Lue M, Marco P.; Hernandez-Caraballo, Edwin A.

    2004-01-01

    The technique of total reflection X-ray fluorescence (TXRF) is well suited for the direct analysis of biological samples due to the low matrix interferences and simultaneous multi-element nature. Nevertheless, biological organic samples are frequently analysed after digestion procedures. The direct determination of analytes requires shorter analysis time, low reactive consumption and simplifies the whole analysis process. On the other hand, the biological/clinical samples are often available in minimal amounts and routine studies require the analysis of large number of samples. To overcome the difficulties associated with the analysis of organic samples, particularly of solid ones, different procedures of sample preparation and calibration to approach the direct analysis have been evaluated: (1) slurry sampling, (2) Compton peak standardization, (3) in situ microwave digestion, (4) in situ chemical modification and (5) direct analysis with internal standardization. Examples of analytical methods developed by our research group are discussed. Some of them have not been previously published, illustrating alternative strategies for coping with various problems that may be encountered in the direct analysis by total reflection X-ray fluorescence spectrometry

  6. Chlorine determination in (U, Pu)C fuel by total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Misra, Nand Lal; Dhara, Sangita; Mudher, Khush Dev Singh; Aggarwal, Suresh K.; Thakur, Uday Kumar; Shah, Dipti; Sawant, R.M.; Ramakumar, K.L.

    2007-01-01

    A Total Reflection X-ray Fluorescence (TXRF) method for the determination of chlorine in (U,Pu)C has been developed. The method involves calibration of the instrument with standard solutions and validation of TXRF determination of chlorine using synthetic standard solutions. Cl K α line excited with W L α source was used for TXRF determinations of chlorine. Chlorine present in trace amounts in (U,Pu)C samples was first separated by pyro hydrolysis. The evolved chlorine, in form of HCl, was collected in 5 mM NaOH solution. This solution was analyzed for chlorine by Total Reflection X-ray Fluorescence Spectrometry using cobalt as an internal standard. The TXRF detection limit of chlorine was found to be 3.6 pg with sample size of 30 μL. In order to assess the applicability of TXRF method for chlorine determinations in other nuclear materials, one U 3 O 8 trace element standard was also analyzed for chlorine in similar way. The precision of the method was found to be 25% (1 σ) at ng level in most of the cases. (author)

  7. Determination of carbon in natural freshwater biofilms with total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ovari, M.; Streli, C.; Wobrauschek, P.; Zaray, Gy.

    2009-01-01

    There is a growing interest in determination of low Z elements, i.e., carbon to phosphorus, in biological samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). Biofilms can be used for biomonioring purposes in the aquatic environment. Besides the trace metals, especially the determination of the carbon content is important for the better understanding of the early stage of biofilm formation. For this, an ATI low Z spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a Si(Li) detector with ultra thin window was used. Biofilms were grown on two different artificial supports (granite and plexiglass), freeze dried, suspended in high purity water and analyzed. As an internal standard the natural titanium content of the biofilms was used. The accuracy of the method was checked by total carbon measurement using a combusting carbon analyzer.

  8. Determination of carbon in natural freshwater biofilms with total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ovari, M. [Department of Analytical Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary)], E-mail: ovari@chem.elte.hu; Streli, C.; Wobrauschek, P. [Atominstitut of the Austrian Universities, TU-Wien, Stadionallee 2, A-1020, Wien (Austria); Zaray, Gy. [Department of Analytical Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary); Cooperative Research Centre of Environmental Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary)

    2009-08-15

    There is a growing interest in determination of low Z elements, i.e., carbon to phosphorus, in biological samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). Biofilms can be used for biomonioring purposes in the aquatic environment. Besides the trace metals, especially the determination of the carbon content is important for the better understanding of the early stage of biofilm formation. For this, an ATI low Z spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a Si(Li) detector with ultra thin window was used. Biofilms were grown on two different artificial supports (granite and plexiglass), freeze dried, suspended in high purity water and analyzed. As an internal standard the natural titanium content of the biofilms was used. The accuracy of the method was checked by total carbon measurement using a combusting carbon analyzer.

  9. Comparison of conventional and total reflection excitation geometry for fluorescence X-ray absorption spectroscopy on droplet samples

    International Nuclear Information System (INIS)

    Falkenberg, G.; Pepponi, G.; Streli, C.; Wobrauschek, P.

    2003-01-01

    X-ray absorption fine structure (XAFS) experiments in fluorescence mode have been performed in total reflection excitation geometry and conventional 45 deg. /45 deg. excitation/detection geometry for comparison. The experimental results have shown that XAFS measurements are feasible under normal total reflection X-ray fluorescence (TXRF) conditions, i.e. on droplet samples, with excitation in grazing incidence and using a TXRF experimental chamber. The application of the total reflection excitation geometry for XAFS measurements increases the sensitivity compared to the conventional geometry leading to lower accessible concentration ranges. However, XAFS under total reflection excitation condition fails for highly concentrated samples because of the self-absorption effect

  10. Elemental concentration analysis in prostate tissues using total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Leitão, R.G.; Palumbo, A.; Souza, P.A.V.R.; Pereira, G.R.; Canellas, C.G.L.; Anjos, M.J.; Nasciutti, L.E.; Lopes, R.T.

    2014-01-01

    Prostate cancer (PCa) currently represents the second most prevalent malignant neoplasia in men, representing 21% of all cancer cases. Benign Prostate Hyperplasia (BPH) is an illness prevailing in men above the age of 50, close to 90% after the age of 80. The prostate presents a high zinc concentration, about 10-fold higher than any other body tissue. In this work, samples of human prostate tissues with cancer, BPH and normal tissue were analyzed utilizing total reflection X-ray fluorescence spectroscopy using synchrotron radiation technique (SR-TXRF) to investigate the differences in the elemental concentrations in these tissues. SR-TXRF analyses were performed at the X-ray fluorescence beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo. It was possible to determine the concentrations of the following elements: P, S, K, Ca, Fe, Cu, Zn and Rb. By using Mann–Whitney U test it was observed that almost all elements presented concentrations with significant differences (α=0.05) between the groups studied. - Highlights: ► Prostate cancer is the most frequently diagnosed form of cancer in men. ► Intracellular Zn is correlated with proliferation, differentiation, or apoptosis. ► The prostate gland accumulate high concentration of Zn. ► SR-TXRF is a technique widely used in the analysis of low concentration in samples

  11. Total reflection x-ray analysis of metals in blood samples

    International Nuclear Information System (INIS)

    Nakamura, Takuya; Matsui, Hiroshi; Kawamata, Masaya

    2009-01-01

    The sample preparation for TXRF (total reflection X-ray fluorescence) quantitative analysis of trace elements in human blood samples was investigated. In the TXRF analysis, a solution sample is dropped and dried on a flat substrate, and then the dried residue is measured. In this case, the dried residue should be flat not to disturb X-ray total reflection on the substrate. In addition, it is required to simply measure the whole blood sample by TXRF method, although a serum is analyzed in many cases. Thus, we studied the optimum conditions of the sample preparation of the whole blood by adding the pure water to apply Hemolysis phenomenon, where blood cells are destroyed due to different of the osmotic pressure, leading to flat residue. It was found that the best S/B ratio was obtained when the whole blood was diluted 8 times with pure water. Moreover, it was investigated the influence of the surface chemical condition of the glass substrate on the shape of the dried reside of the blood sample. When the surface of the glass substrate was hydrophilic, the shape of the dried residues was not uniform, as a result, the quantitative data of TXRF analysis gave a large deviation. On the other hand, when the surface of the glass was hydrophobic, the shape of the residue was almost uniform, as a result, a good reproducibility was obtained. Another problem was an outer ring of the dried residue of the blood. This uneven ring absorbs the primary X-rays, caused to low determined quantitative data. Thus, we tried the heating way of the dropped blood sample at a high temperature of 200 degrees. In this case, the blood sample was dried immediately, and a flat homogeneous dried residue was obtained without the outer ring. Using the optimized conditions for sample preparation, human blood sample was quantitatively measured by TXRF and ICP-AES. A good agreement was obtained in TXRF and ICP-AES determinations; however, the measurement of Cl and Br will be an advantage of TXRF, because

  12. Colouration of medieval glass bracelets studied by total reflection x-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Detcheva, Albena; Velinova, Ralitsa; Ivanova, Elisaveta; Jordanov, Juri; Karadjov, Metody

    2014-01-01

    The contents of 3d-transition metals (Ti, V, Cr, Mn, Fe, Co, Ni, Cu and Zn) in fragments of medieval glass bracelets, found in the necropolis of Stambolovo and the castle of Mezek, Bulgaria, were determined by total reflection X-ray fluorescence (TXRF) analysis using gallium as internal standard. The samples were analysed as slurries in Triton X 114. The experimental parameters: grain size of the glass sample, concentrations of glass sample, Triton X114 and internal standard in the slurry, volume of the slurry aliquot taken for analysis, as well as the excitation time, were optimised. For method validation the certified reference material BAM-S005 Type A soda-lime glass was used. It was proven that the elements Co, Mn and Fe are responsible for colour generation in the investigated glass samples. The precision of the determinations is characterised by an RSD in the range 3–11%

  13. Impurities determination in uranium eluates by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Vazquez, Cristina; Bellavigna, Horacio J.; Eppis, Maria R.; Ramella, Jose L.

    1999-01-01

    The chemical control of impurities in nuclear materials is indispensable in order to assure an efficient operation of the reactors. The maximum concentration admitted depends of the elements and in most cases are in the parts per billion range. Conventional analytical methods require a pre-concentration treatment of the sample and a previous separation of the matrix (uranium). This paper investigates the use of the total reflection X-ray fluorescence as an alternative methodology for the determination of impurities in nuclear materials, namely K, Ca, Ti, Cr, Mn, Fe, Ni, Cu and As. The detection limits obtained were in the range of 0.1 to 20 ng/ml for a 1000 seconds counting time. (author)

  14. Metals determination in coffee sample by total reflection X-ray fluorescence analysis (TXRF)

    International Nuclear Information System (INIS)

    Vives, Ana Elisa Sirito de

    2005-01-01

    The objective of this study was to evaluate the inorganic concentration in five brands of coffee, three of them nationally marketed and the others of an exportation kind. The samples were prepared by infusion with deionized water. To carry out the calibration, standard solutions were prepared with different concentrations of Al, Si, K, Ca, Ti, Cr, Fe, Ni, Zn and Se. The measurements were carried out using a white beam of synchrotron radiation for excitation and a Si (Li) semiconductor detector for detection. By employing Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF) it was possible to evaluate the concentrations of P, S, Cl, K, Ca, Mn, Fe, Cu, Zn, Rb and Ba. The detection limits for 300 s counting time were in the range of 0.03 (Ca) to 30 ng.g -1 (Rb), respectively. (author)

  15. Multielemental analysis in Brazilian cigarettes using total reflection X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T.; Moreira, Silvana

    2005-01-01

    In order to identify major and trace elements in conventional and light Brazilian cigarettes, Total Reflection X-Ray Fluorescence with Synchrotron Radiation (SR-TXRF) was used. The fluorescence measurements were carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo. This technique enables detection limit is in the ngg -1 range, which is very useful in elemental tobacco smoke analysis, since it presents most of its elements at a trace level. The major elements identified in tobacco samples were: S, Cl, K, Ca, Mn, Fe and Cd, and the trace elements were: Ti, Cr, Ni, Cu, Zn, Br, Rb, Sr and Ba. However in tobacco smoke samples, there were only two major elements: K and Ca, the others were present a trace level. The rate transfer of tobacco to tobacco smoke was about 2.5 % for all elements studied. (author)

  16. Recent trends in total reflection X-ray fluorescence spectrometry for biological applications

    International Nuclear Information System (INIS)

    Szoboszlai, Norbert; Polgari, Zsofia; Mihucz, Victor G.; Zaray, Gyula

    2009-01-01

    This review is focused on the application of total reflection X-ray fluorescence (TXRF) spectrometry in the field of biological research. In the last decade, most papers were published by authors who applied laboratory-scale TXRF equipments. The application of synchrotron radiation as excitation source (SR-TXRF) shows a slowly increasing tendency. In the cited papers the micro-, trace and multielement capability of these TXRF techniques was demonstrated in the clinical and medical laboratory practice, as well as in various plant physiological studies. For speciation of elements in biological matrices, the TXRF was used as element specific detector following an off-line separation step (e.g., thin layer chromatography, high performance liquid chromatography), however, these off-line methods are not competitive with the on-line coupled HPLC-inductively coupled plasma mass spectrometry

  17. Total-reflection X-ray fluorescence: An alternative tool for the analysis of magnetic ferrofluids

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Servicio Interdepartamental de Investigacion (SIdI), Facultad de Ciencias, Universidad Autonoma de Madrid, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Costo, R.; Morales, M.P.; Bomati-Miguel, O.; Veintemillas-Verdaguer, S. [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049, Madrid (Spain)

    2008-12-15

    This work presents the first application of the total-reflection X-ray fluorescence (TXRF) to the compositional study of magnetic ferrofluids. With the aims of validating the best analytical conditions and also, limitations of the TXRF in the compositional study of these materials, an alternative empirical method, based in the use of angle-dependence TXRF (AD-TXRF) measurements, is proposed. Three kinds of ferromagnetic nanoparticles, with different morphologies, have been studied. The techniques of inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectroscopy (ICP-OES) have been used to validate the TXRF results. In contrast with the plasma techniques, the developed TXRF procedure need not of previous chemical acid digestion. Additionally, two procedures of magnetic nanoparticles synthesis, co-precipitation and laser-pyrolysis, have been checked for the contaminants trace metals Zn, Mn and Cr. It has been found that the method of laser-pyrolysis produces nanoparticles of higher purity.

  18. Fundamental quantification procedure for total reflection X-ray fluorescence spectra analysis and elements determination

    International Nuclear Information System (INIS)

    Wegrzynek, D.; Holynska, B.

    1997-01-01

    A method for the determination of the concentrations of elements in particulate-like samples measured in total reflection geometry is proposed. In the proposed method the fundamental parameters are utilized for calculating the sensitivities of elements and an internal standard is used to account for the unknown mass per unit area of a sample and geometrical constant of the spectrometer. The modification of the primary excitation spectrum on its way to a sample has been taken into consideration. The concentrations of the elements to be determined are calculated simultaneously with the spectra deconvolution procedure. In the process of quantitative analysis the intensities of all X-ray peaks corresponding to K and L-series lines present in the analyzed spectrum are taken into account. (Author)

  19. First Total Reflection X-Ray Fluorescence round-robin test of water samples: Preliminary results

    Energy Technology Data Exchange (ETDEWEB)

    Borgese, Laura; Bilo, Fabjola [Chemistry for Technologies Laboratory, University of Brescia, Brescia (Italy); Tsuji, Kouichi [Graduate School of Engineering, Osaka City University, Osaka (Japan); Fernández-Ruiz, Ramón [Servicio Interdepartamental de Investigación (SIdI), Laboratorio de TXRF, Universidad Autónoma de Madrid, Madrid (Spain); Margui, Eva [Department of Chemistry, University of Girona, Girona (Spain); Streli, Christina [TU Wien, Atominstitut,Radiation Physics, Vienna (Austria); Pepponi, Giancarlo [Fondazione Bruno Kessler, Povo, Trento (Italy); Stosnach, Hagen [Bruker Nano GmbH, Berlin (Germany); Yamada, Takashi [Rigaku Corporation, Takatsuki, Osaka (Japan); Vandenabeele, Peter [Department of Archaeology, Ghent University, Ghent (Belgium); Maina, David M.; Gatari, Michael [Institute of Nuclear Science and Technology, University of Nairobi, Nairobi (Kenya); Shepherd, Keith D.; Towett, Erick K. [World Agroforestry Centre (ICRAF), Nairobi (Kenya); Bennun, Leonardo [Laboratorio de Física Aplicada, Departamento de Física, Universidad de Concepción (Chile); Custo, Graciela; Vasquez, Cristina [Gerencia Química, Laboratorio B025, Centro Atómico Constituyentes, San Martín (Argentina); Depero, Laura E., E-mail: laura.depero@unibs.it [Chemistry for Technologies Laboratory, University of Brescia, Brescia (Italy)

    2014-11-01

    Total Reflection X-Ray Fluorescence (TXRF) is a mature technique to evaluate quantitatively the elemental composition of liquid samples deposited on clean and well polished reflectors. In this paper the results of the first worldwide TXRF round-robin test of water samples, involving 18 laboratories in 10 countries are presented and discussed. The test was performed within the framework of the VAMAS project, interlaboratory comparison of TXRF spectroscopy for environmental analysis, whose aim is to develop guidelines and a standard methodology for biological and environmental analysis by means of the TXRF analytical technique. - Highlights: • The discussion of the first worldwide TXRF round-robin test of water samples (18 laboratories of 10 countries) is reported. • Drinking, waste, and desalinated water samples were tested. • Data dispersion sources were identified: sample concentration, preparation, fitting procedure, and quantification. • The protocol for TXRF analysis of drinking water is proposed.

  20. Metals determination in coffee sample by total reflection X-ray fluorescence analysis (TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Brienza, Sandra Maria Boscolo [ Universidade Metodista de Piracicaba (UNIMEP), Piracicaba, SP (Brazil). Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)]. E-mail: virgilio@cena.usp.br

    2005-07-01

    The objective of this study was to evaluate the inorganic concentration in five brands of coffee, three of them nationally marketed and the others of an exportation kind. The samples were prepared by infusion with deionized water. To carry out the calibration, standard solutions were prepared with different concentrations of Al, Si, K, Ca, Ti, Cr, Fe, Ni, Zn and Se. The measurements were carried out using a white beam of synchrotron radiation for excitation and a Si (Li) semiconductor detector for detection. By employing Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF) it was possible to evaluate the concentrations of P, S, Cl, K, Ca, Mn, Fe, Cu, Zn, Rb and Ba. The detection limits for 300 s counting time were in the range of 0.03 (Ca) to 30 ng.g{sup -1} (Rb), respectively. (author)

  1. Parameter study of self-absorption effects in Total Reflection X-ray Fluorescence-X-ray Absorption Near Edge Structure analysis of arsenic

    International Nuclear Information System (INIS)

    Meirer, F.; Pepponi, G.; Streli, C.; Wobrauschek, P.; Kregsamer, P.; Zoeger, N.; Falkenberg, G.

    2008-01-01

    Total reflection X-ray Fluorescence (TXRF) analysis in combination with X-ray Absorption Near Edge Structure (XANES) analysis is a powerful method to perform chemical speciation studies at trace element levels. However, when measuring samples with higher concentrations and in particular standards, damping of the oscillations is observed. In this study the influence of self-absorption effects on TXRF-XANES measurements was investigated by comparing measurements with theoretical calculations. As(V) standard solutions were prepared at various concentrations and dried on flat substrates. The measurements showed a correlation between the damping of the oscillations and the As mass deposited. A Monte-Carlo simulation was developed using data of the samples shapes obtained from confocal white light microscopy. The results showed good agreement with the measurements; they confirmed that the key parameters are the density of the investigated atom in the dried residues and the shape of the residue, parameters that combined define the total mass crossed by a certain portion of the incident beam. The study presents a simple approach for an a priori evaluation of the self-absorption in TXRF X-ray absorption studies. The consequences for Extended X-ray Absorption Fine Structure (EXAFS) and XANES measurements under grazing incidence conditions are discussed, leading to the conclusion that the damping of the oscillations seems to make EXAFS of concentrated samples non feasible. For XANES 'fingerprint' analysis samples should be prepared with a deposited mass and sample shape leading to an acceptable absorption for the actual investigation

  2. Total reflection x-ray fluorescence spectrometers for multielemental analysis: status of commercial equipment

    International Nuclear Information System (INIS)

    Ayala Jimenez, R.E.

    2000-01-01

    Multi-elemental analysis by total reflection x-ray fluorescence spectrometry has evolved during two decades. At the present there are commercial equipment available for the chemical analysis in all kind of biological and mineral samples. The electronic industry has also been benefited from the scientific and technological developments in the field of TXRF. The basic components of the spectrometers can be summarized as follow: a) excitation source; b) geometric arrangement (optics) for collimation and monochromatization of the primary radiation; c) x-ray detector; d) hardware and software for operation of the instrument, data acquisition and spectral deconvolution to determine the concentrations of the element present in the sample (quantitative analysis). As optional there are manufacturers offering the conventional 45 degrees geometry for direct excitation of bulky liquid or solid samples. Personal communications of the author and the commercial brochures available at the moment of writing this presentation have allowed to list the following type of components used in the TXRF spectrometers for multi-elemental analysis (the devices used in the electronic industry to analyze silicon wafers are excluded). Excitation: high power x-ray tube, output from 1300 to 2000 watts; metal ceramic low power-ray tube, output up to 50 watts. Different anodes are used but molybdenum, tungsten and copper are frequent. The excitation systems can be customized according to the requirements of the laboratory. Detector: Si-Li semi-conductor liquid nitrogen cooled; silicon solid state thermoelectrically cooled (silicon drift detector SDD and Si-PIN diode). Optics: multilayer monochromator of Si-W or Ni-C; double multilayer monochromator. Electronics: spectroscopy amplifier, analog to digital converter adapted to a PC compatible computer with software in Windows environment for the whole operation of the spectrometer and for qualy/quantitative analysis of samples are standards in the

  3. Total reflection X-ray fluorescence analysis of airborne silver nanoparticles from fabrics.

    Science.gov (United States)

    Menzel, Magnus; Fittschen, Ursula Elisabeth Adriane

    2014-03-18

    Ag nanoparticles (NPs) are usually applied to consumer products because of their antimicrobial properties, which are desired in fabrics for sportswear as well as cloth used for cleaning. Hazards to human health from airborne Ag NPs may occur when the NPs are inhaled. NPs are comparable in size to macromolecules and viruses and able to penetrate deep into the lungs, e.g., the alveoli, where they may cause damage to cells and tissue due to their large surface area. In this study, aerosols released form fabrics treated with Ag NPs were collected using a low pressure Berner impactor and analyzed with total reflection X-ray fluorescence (TXRF). We found that the Ag NPs are released primarily in the form of larger particles, mainly 0.13-2 μm, probably attached to fiber material. Using an electron micro probe, single particles could be identified. The detection of backscattered electrons suggests small spots on the particle consist of a heavier element, which most likely is Ag, although the signal in energy-dispersive X-ray spectroscopy (EDX) was below the lower limit of detection (LOD). To achieve LODs necessary for Ag determination, Ar peaks were eliminated by a nitrogen atmosphere provided by the "Picofox-box". This enables linear calibration and quantification of Ag. The LOD was calculated at 0.2 ng (2.0 ppb). Following the TXRF and scanning electron microscopy (SEM)/EDX analysis, the aerosol samples were dissolved in nitric acid and analyzed with ICPMS to successfully confirm the results obtained by the TXRF measurements.

  4. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, Ursula Elisabeth Adriane, E-mail: ursula.fittschen@chemie.uni-hamburg.de [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Menzel, Magnus [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Scharf, Oliver [IfG Institute for Scientific Instruments GmbH, Berlin (Germany); Radtke, Martin; Reinholz, Uwe; Buzanich, Günther [BAM Federal Institute of Materials Research and Testing, Berlin (Germany); Lopez, Velma M.; McIntosh, Kathryn [Los Alamos National Laboratory, Los Alamos, NM (United States); Streli, Christina [Atominstitut, TU Wien, Vienna (Austria); Havrilla, George Joseph [Los Alamos National Laboratory, Los Alamos, NM (United States)

    2014-09-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. - Highlights: • Use of a color X-ray camera and drop on demand printing to diagnose X-ray shading • Specimens were obtained uniform and well-defined in shape and concentration by printing. • Direct visualization and determination of shading in such specimens using the camera.

  5. Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera

    International Nuclear Information System (INIS)

    Fittschen, Ursula Elisabeth Adriane; Menzel, Magnus; Scharf, Oliver; Radtke, Martin; Reinholz, Uwe; Buzanich, Günther; Lopez, Velma M.; McIntosh, Kathryn; Streli, Christina; Havrilla, George Joseph

    2014-01-01

    Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by “drop on demand” technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. - Highlights: • Use of a color X-ray camera and drop on demand printing to diagnose X-ray shading • Specimens were obtained uniform and well-defined in shape and concentration by printing. • Direct visualization and determination of shading in such specimens using the camera

  6. First combined total reflection X-ray fluorescence and grazing incidence X-ray absorption spectroscopy characterization of aeolian dust archived in Antarctica and Alpine deep ice cores

    Energy Technology Data Exchange (ETDEWEB)

    Cibin, G. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxon OX110DE (United Kingdom); IMONT/EIM, Ente Italiano della Montagna, P.za dei Caprettari 70, 00176 Roma (Italy); Universita' degli Studi di Roma Tre, Dipartimento di Scienze Geologiche, L.go S. Leonardo Murialdo 1, 00146 Roma (Italy)], E-mail: giannantonio.cibin@diamond.ac.uk; Marcelli, A. [INFN - Laboratori Nazionali di Frascati, P.O. Box 13, 00044 Frascati (Roma) (Italy); Maggi, V. [Universita degli Studi di Milano-Bicocca, Dipartimento di Scienze dell' Ambiente e del Territorio, Piazza della Scienza 1, 20126 Milano (Italy); Sala, M. [Universita degli Studi di Milano-Bicocca, Dipartimento di Scienze dell' Ambiente e del Territorio, Piazza della Scienza 1, 20126 Milano (Italy); Universita degli Studi di Milano, Dipartimento di Scienze della Terra ' A. Desio' , Sez. Mineralogia, Via Mangiagalli 34, 20133 Milano (Italy); Marino, F.; Delmonte, B. [Universita degli Studi di Milano-Bicocca, Dipartimento di Scienze dell' Ambiente e del Territorio, Piazza della Scienza 1, 20126 Milano (Italy); Albani, S. [Universita degli Studi di Milano-Bicocca, Dipartimento di Scienze dell' Ambiente e del Territorio, Piazza della Scienza 1, 20126 Milano (Italy); Universita degli Studi di Siena, Dottorato in Scienze Polari, via Laterina 8, 53100 Siena (Italy); Pignotti, S. [IMONT/EIM, Ente Italiano della Montagna, P.za dei Caprettari 70, 00176 Roma (Italy)

    2008-12-15

    Aeolian mineral dust archived in polar and mid latitude ice cores represents a precious proxy for assessing environmental and climatic variations at different timescales. In this respect, the identification of dust mineralogy plays a key role. In this work we performed the first preliminary X-ray absorption spectroscopy (XAS) experiments on mineral dust particles extracted from Antarctic and from Alpine firn cores using grazing incidence geometry at the Fe K-edge. A dedicated high vacuum experimental chamber was set up for normal-incidence and total-reflection X-Ray Fluorescence and Absorption Spectroscopy analyses on minor amounts of mineral materials at the Stanford Synchrotron Radiation Laboratory. Results show that this experimental technique and protocol allows recognizing iron inclusion mineral fraction on insoluble dust in the 1-10 {mu}g range.

  7. First combined total reflection X-ray fluorescence and grazing incidence X-ray absorption spectroscopy characterization of aeolian dust archived in Antarctica and Alpine deep ice cores

    International Nuclear Information System (INIS)

    Cibin, G.; Marcelli, A.; Maggi, V.; Sala, M.; Marino, F.; Delmonte, B.; Albani, S.; Pignotti, S.

    2008-01-01

    Aeolian mineral dust archived in polar and mid latitude ice cores represents a precious proxy for assessing environmental and climatic variations at different timescales. In this respect, the identification of dust mineralogy plays a key role. In this work we performed the first preliminary X-ray absorption spectroscopy (XAS) experiments on mineral dust particles extracted from Antarctic and from Alpine firn cores using grazing incidence geometry at the Fe K-edge. A dedicated high vacuum experimental chamber was set up for normal-incidence and total-reflection X-Ray Fluorescence and Absorption Spectroscopy analyses on minor amounts of mineral materials at the Stanford Synchrotron Radiation Laboratory. Results show that this experimental technique and protocol allows recognizing iron inclusion mineral fraction on insoluble dust in the 1-10 μg range

  8. Collection of airborne particulate matter for a subsequent analysis by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Klockenkaemper, R.; Bayer, H.; Bohlen, A. von; Schmeling, M.; Klockow, D.

    1995-01-01

    The collection of airborne particulate matter by filtration and impaction was adapted to total reflection X-ray fluorescence analysis (TXRF). Cellulose nitrate filters were used for collecting in a Berner impactor. Single filter spots were punched out, placed on quartz-glass carriers, dissolved by tetrahydrofuran and re-precipitated prior to element determinations by TXRF. In a Battelle-type impactor, airborne dust was collected on Plexiglass carriers coated with medical Vaseline. The loaded carriers were directly analyzed by TXRF. In both cases, quantification was simply performed by the addition of an internal standard after sampling. Impactors were made of a suitable material in order to investigate high blank values, collection losses and memory effects. It could be shown that stainless steel, even coated with TiN, is less suitable and should be avoided as an impactor material. Although aluminum is partly recommendable, titanium and the polymer Makrolon are quite appropriate. By using an impactor made of these materials, a reliable multielement determination in airborne dust is made possible with low detection limits as low as 1 ng/m 3 and a satisfactory repeatability of a few %. Short sampling times of only 1 h or less can be realized. The total procedure is simple and time-saving, and can be recommended for routine investigations of airborne particulate matter. (author)

  9. The effect of surface texture on total reflection of neutrons and X-rays from modified interfaces

    DEFF Research Database (Denmark)

    Goldar, A.; Roser, S.J.; Hughes, A.

    2002-01-01

    X-ray and neutron scattering from macroscopically rough surfaces and interfaces is considered and a new method of analysis based on the variation of the shape of the total reflection edge in the reflectivity profile is proposed. It was shown that in the limit that the correlation length and the h......X-ray and neutron scattering from macroscopically rough surfaces and interfaces is considered and a new method of analysis based on the variation of the shape of the total reflection edge in the reflectivity profile is proposed. It was shown that in the limit that the correlation length...... and the height of the surface roughness are larger than the wavelength (at least 100 times bigger) of the incoming beam, the total reflection edge in the reflection profile becomes rounded. This technique allows direct analysis of the variation of the reflectivity pro le in terms of the structure of the surface...

  10. Investigation of polyelectrolytes by total reflection x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Varga, I.; Nagy, M.

    2000-01-01

    Water soluble polyelectrolyte samples containing mono-, bi- and trivalent metal ions were investigated without any pretreatment. Acid digestion of linear polymers may lead to a product insoluble in water so the digestion has to be avoided. The aim of this paper was the determination of analytical characteristics and limitations of the total reflection x-ray fluorescence (TXRF) analysis for poly (vinylalcohol-vinylsulphate) salts and poly (acrylic acid, acrylamide) copolymers containing the following cations: K + , Cs + , Ba 2+ , Cu 2+ and La 3+ . On the basis of our results efficiency of ion-exchange during preparation of polyelectrolytes and stoichiometry of the end-product were determined. TXRF results were compared with data gained by inductively coupled plasma atomic emission spectrometry (ICP-AES) measurements except in the case of Cs + which has poor sensitivity in ICP-AES. Good agreement was found between the results of the two techniques and calculations from titrimetric data. Concentration of Li + and Mg 2+ in polymer samples was measured by ICP-AES. In majority of cases film-like dry residues of aqueous solutions of polyelectrolytes can be characterized by homogeneous spatial distribution of metal ions within the organic matrix. This is because the migration of the ions is hindered during drying process. Determination of metals in polyelectrolyte films by TXRF is quite ideal as model for analysis of plant, animal or human tissues which is a frequent task in environmental and inorganic biomedical analytical chemistry. (author)

  11. Synchrotron radiation total reflection x-ray fluorescence analysis; of polymer coated silicon wafers

    International Nuclear Information System (INIS)

    Brehm, L.; Kregsamer, P.; Pianetta, P.

    2000-01-01

    It is well known that total reflection x-ray fluorescence (TXRF) provides an efficient method for analyzing trace metal contamination on silicon wafer surfaces. New polymeric materials used as interlayer dielectrics in microprocessors are applied to the surface of silicon wafers by a spin-coating process. Analysis of these polymer coated wafers present a new challenge for TXRF analysis. Polymer solutions are typically analyzed for bulk metal contamination prior to application on the wafer using inductively coupled plasma mass spectrometry (ICP-MS). Questions have arisen about how to relate results of surface contamination analysis (TXRF) of a polymer coated wafer to bulk trace analysis (ICP-MS) of the polymer solutions. Experiments were done to explore this issue using synchrotron radiation (SR) TXRF. Polymer solutions were spiked with several different concentrations of metals. These solutions were applied to silicon wafers using the normal spin-coating process. The polymer coated wafers were then measured using the SR-TXRF instrument set-up at the Stanford Synchrotron Radiation Laboratory (SSRL). Several methods of quantitation were evaluated. The best results were obtained by developing calibration curves (intensity versus ppb) using the spiked polymer coated wafers as standards. Conversion of SR-TXRF surface analysis results (atoms/cm 2 ) to a volume related concentration was also investigated. (author)

  12. Multielement analysis of aerosol samples by X-ray fluorescence analysis with totally reflecting sample holders

    International Nuclear Information System (INIS)

    Ketelsen, P.; Knoechel, A.

    1984-01-01

    Aerosole samples on filter support were analyzed using the X-ray flourescence analytical method (Mo excitation) with totally reflecting sample carrier (TXFA). Wet decomposition of the sample material with HNO 3 in an enclosed system and subsequent sample preparation by evaporating an aliquot of the solution on the sample carrier yields detection limits up to 0.3 ng/cm 2 . The reproducibilities of the measurements of the elements K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Ba and Pb lie between 5 and 25%. Similar detection limits and reproducibilities are obtained, when low-temperature oxygen plasma is employed for the direct ashing of the homogenously covered filter on the sample carrier. For the systematic loss of elements both methods were investigated with radiotracers as well as with inactive techniques. A comparison of the results with those obtained by NAA, AAS and PIXE shows good agreement in most cases. For the bromine determination and the fast coverage of the main elements a possibility for measuring the filter membrane has been indicated, which neglects the ashing step. The corresponding detection limits are up to 3 ng/cm 2 . (orig.) [de

  13. Characterization and classification of spirituous beverages by total reflection x-ray fluorescence

    International Nuclear Information System (INIS)

    Davila, E.G. de; Lue-Meru, M.P.; Capote, T.; Greaves, E.

    2000-01-01

    The total reflection x-ray fluorescence (TXRF) technique was applied for the multi-elemental analysis of spirituous beverages like rum, cocuy (typical spirituous beverage in Venezuela), whiskey and wine, in order to classify the samples by product processing and geographical origin by chemometric analysis. Special attention was paid to the cocuy samples, since there is a lack of quality control of this beverage, mainly due to the home-made product processing. The use of the Compton peak information was evaluated for the determination of organic content in samples. In the specifically case of cocuy samples the Compton peak area was correlated to the ash content for detection of adulteration with sugar syrup. Cocuy samples were also analyzed using gas chromatography, for pH, acidity, ash content and refractometry, in order to develop the recognition pattern. The TXRF analysis was carried out in a Canberra spectrometer, using the K α-line of a Motube, by a direct procedure previously developed. The analysis of the data was done by using principal components analysis and a confidence test. The results show that TXRF and chemometric analysis is a useful tool for quality control of spirituous beverages, not only concerning to metal content, but also in the evaluation of sugar and non volatile organic content. (author)

  14. Characterization and classification of spirituous beverages by total reflection x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Davila, E.G. de [Univerisdad Centroccidental Lisandro Alvarado, Decanato de Agronomia, Dpto. de Quimica y Suelos. Nucleo Tarabana, cabudare, Edo. Lara (Venezuela); Lue-Meru, M P; Capote, T [Univerisdad Centroccidental Lisandro Alvarado, Decanato de Agronomia, Dpto. de Quimica y Suelos. Nucleo Tarabana, Cabudare, Edo. Lara (Venezuela); Universidad Simon Bolivar, Dpto. de Quimica, Lab. Espectroscopia Atomica, Sartenejas, Baruta, Edo. Miranda (Venezuela); Greaves, E [Universidad Simon Bolivar, Dpto. de Fisica, Sartenejas, Baruta, Edo. Miranda (Venezuela)

    2000-07-01

    The total reflection x-ray fluorescence (TXRF) technique was applied for the multi-elemental analysis of spirituous beverages like rum, cocuy (typical spirituous beverage in Venezuela), whiskey and wine, in order to classify the samples by product processing and geographical origin by chemometric analysis. Special attention was paid to the cocuy samples, since there is a lack of quality control of this beverage, mainly due to the home-made product processing. The use of the Compton peak information was evaluated for the determination of organic content in samples. In the specifically case of cocuy samples the Compton peak area was correlated to the ash content for detection of adulteration with sugar syrup. Cocuy samples were also analyzed using gas chromatography, for pH, acidity, ash content and refractometry, in order to develop the recognition pattern. The TXRF analysis was carried out in a Canberra spectrometer, using the K {alpha}-line of a Motube, by a direct procedure previously developed. The analysis of the data was done by using principal components analysis and a confidence test. The results show that TXRF and chemometric analysis is a useful tool for quality control of spirituous beverages, not only concerning to metal content, but also in the evaluation of sugar and non volatile organic content. (author)

  15. Metal ions diffusion through polymeric matrices: A total reflection X-ray fluorescence study

    International Nuclear Information System (INIS)

    Boeykens, S.; Caracciolo, N.; D'Angelo, M.V.; Vazquez, C.

    2006-01-01

    This work proposes the use of X-ray fluorescence with total reflection geometry to explore the metal ions transport in aqueous hydrophilic polymer solutions. It is centered in the study of polymer concentration influence on ion diffusion. This subject is relevant to various and diverse applications, such as drug controlled release, microbiologic corrosion protection and enhanced oil recovery. It is anticipated that diffusion is influenced by various factors in these systems, including those specific to the diffusing species, such as charge, shape, molecular size, and those related to the structural complexity of the matrix as well as any specific interaction between the diffusing species and the matrix. The diffusion of nitrate salts of Ba and Mn (same charge, different hydrodynamic radii) through water-swollen polymeric solutions and gels in the 0.01% to 1% concentration ranges was investigated. The measurements of the metal concentration were performed by TXRF analysis using the scattered radiation by the sample as internal standard. Results are discussed according to different physical models for solute diffusion in polymeric solutions

  16. Total reflection X-ray fluorescence as a tool for food screening

    Science.gov (United States)

    Borgese, Laura; Bilo, Fabjola; Dalipi, Rogerta; Bontempi, Elza; Depero, Laura E.

    2015-11-01

    This review provides a comprehensive overview of the applications of total reflection X-ray fluorescence (TXRF) in the field of food analysis. Elemental composition of food is of great importance, since food is the main source of essential, major and trace elements for animals and humans. Some potentially toxic elements, dangerous for human health may contaminate food, entering the food chain from the environment, processing, and storage. For this reason the elemental analysis of food is fundamental for safety assessment. Fast and sensitive analytical techniques, able to detect major and trace elements, are required as a result of the increasing demand on multi-elemental information and product screening. TXRF is suitable for elemental analysis of food, since it provides simultaneous multi-elemental identification in a wide dynamic range of concentrations. Several different matrices may be analyzed obtaining results with a good precision and accuracy. In this review, the most recent literature about the use of TXRF for the analysis of food is reported. The focus is placed on the applications within food quality monitoring of drinks, beverages, vegetables, fruits, cereals, animal derivatives and dietary supplements. Furthermore, this paper provides a critical outlook on the developments required to transfer these methods from research to the industrial and analytical laboratories contexts.

  17. Sample preparation for total reflection X-ray fluorescence analysis using resist pattern technique

    Science.gov (United States)

    Tsuji, K.; Yomogita, N.; Konyuba, Y.

    2018-06-01

    A circular resist pattern layer with a diameter of 9 mm was prepared on a glass substrate (26 mm × 76 mm; 1.5 mm thick) for total reflection X-ray fluorescence (TXRF) analysis. The parallel cross pattern was designed with a wall thickness of 10 μm, an interval of 20 μm, and a height of 1.4 or 0.8 μm. This additional resist layer did not significantly increase background intensity on the XRF peaks in TXRF spectra. Dotted residue was obtained from a standard solution (10 μL) containing Ti, Cr, Ni, Pb, and Ga, each at a final concentration of 10 ppm, on a normal glass substrate with a silicone coating layer. The height of the residue was more than 100 μm, where self-absorption in the large residue affected TXRF quantification (intensity relative standard deviation (RSD): 12-20%). In contrast, from a droplet composed of a small volume of solution dropped and cast on the resist pattern structure, the obtained residue was not completely film but a film-like residue with a thickness less than 1 μm, where self-absorption was not a serious problem. In the end, this sample preparation was demonstrated to improve TXRF quantification (intensity RSD: 2-4%).

  18. Multielemental analysis in cigarettes using total reflection X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Barbosa, R.F.; Anjos, M.J. dos; Jesus, E.F.O. de; Lopes, R.T.; Moreira, S.

    2008-01-01

    Full text: It is well known that trace elements have important ejects in the life processes. Some of these elements are toxic for the human even at a very low level of intake. It is known that tobacco plant easily absorbs the heavy metals from the soil, especially Cd and Ni, accumulating them in its leaves. Part of these metals are transferred from tobacco to human body where they will be accumulated and damage some organs, mainly kidneys and liver. In this way, cigarettes are responsible for the death of millions of people in the world, about one death every eight seconds. The aim of this work was to determine the elemental concentrations of ten different elements in tobacco of Brazilian cigarettes used Total Reflection X-Ray Fluorescence with Synchrotron Radiation method. The fluorescence measurements were carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo. A qualitative analysis of spectral peaks showed that the samples contained potassium, calcium, titanium, chromium, manganese, iron, copper, rubidium and strontium. Among these elements, calcium, potassium and iron presented the highest concentrations. There was a wide range in the elemental concentrations in the tobacco, due various factors, such as agricultural practices, soil characteristics, climatic conditions and plant varieties. Our results are in good concern with the results reported by the scientific literature

  19. The role of total-reflection x-ray fluorescence in atomic spectroscopy

    International Nuclear Information System (INIS)

    Toelg, G.; Klockenkaemper, R.

    1993-01-01

    Total-reflection X-ray fluorescence (TXRF) is a universal and economic method for the simultaneous determination of elements with atomic numbers > 11 down to the lower pg-level. It is a microanalytical tool for the analysis of small sample amounts placed on flat carriers and for contaminations on flat sample surfaces. Analyses of stratified near-surface layers are made possible by varying the incident angle of the primary beam in the region of total-reflection. This non-destructive method is especially suitable for thin layers of a few nanometres, deposited on wafer material although not usable as a microprobe method with a high lateral resolution. Furthermore, depth profiles of biological samples can be recorded by means of microtome sectioning of only a few micrometres, as, for example in the gradient analysis of human organs. In addition to micro- and surface-layer analysis, TXRF is effectively applied to element trace analysis. Homogeneous solutions, for example aqueous solutions, high-purity acids or body fluids, are pipetted onto carriers and, after evaporation, the dry residues are analyzed directly down to the pg/ml region. Particularly advantageous is the absence of matrix effects, so that an easy calibration can be carried out by adding a single internal standard element. A digestion or separation step preceding the actual determination becomes necessary if a more complex matrix is to be analysed or especially low detection limits have to be reached. A critical evaluation of the recent developments in atomic spectroscopy places TXRF in a leading position. Its outstanding features compete with those of e.g. electrothermal atomic absorption spectrometry (ETAAS), microwave induced plasma optical emission spectroscopy (MIP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) in the field of micro- and trace analysis and with Rutherford backscattering (RBS) and secondary ion mass spectrometry (SIMS) in the surface-layer analysis. (author)

  20. Synchrotron Radiation Total Reflection X-ray Fluorescence Spectroscopy for Microcontamination Analysis on Silicon Wafer Surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Takaura, Norikatsu

    1997-10-01

    As dimensions in state-of-the-art CMOS devices shrink to less than 0.1 pm, even low levels of impurities on wafer surfaces can cause device degradation. Conventionally, metal contamination on wafer surfaces is measured using Total Reflection X-Ray Fluorescence Spectroscopy (TXRF). However, commercially available TXRF systems do not have the necessary sensitivity for measuring the lower levels of contamination required to develop new CMOS technologies. In an attempt to improve the sensitivity of TXRF, this research investigates Synchrotron Radiation TXRF (SR TXRF). The advantages of SR TXRF over conventional TXRF are higher incident photon flux, energy tunability, and linear polarization. We made use of these advantages to develop an optimized SR TXRF system at the Stanford Synchrotron Radiation Laboratory (SSRL). The results of measurements show that the Minimum Detection Limits (MDLs) of SR TXRF for 3-d transition metals are typically at a level-of 3x10{sup 8} atoms/cm{sup 2}, which is better than conventional TXRF by about a factor of 20. However, to use our SR TXRF system for practical applications, it was necessary to modify a commercially available Si (Li) detector which generates parasitic fluorescence signals. With the modified detector, we could achieve true MDLs of 3x10{sup 8} atoms/cm{sup 2} for 3-d transition metals. In addition, the analysis of Al on Si wafers is described. Al analysis is difficult because strong Si signals overlap the Al signals. In this work, the Si signals are greatly reduced by tuning the incident beam energy below the Si K edge. The results of our measurements show that the sensitivity for Al is limited by x-ray Raman scattering. Furthermore, we show the results of theoretical modeling of SR TXRF backgrounds consisting of the bremsstrahlung generated by photoelectrons, Compton scattering, and Raman scattering. To model these backgrounds, we extended conventional theoretical models by taking into account several aspects particular

  1. Determination of lead in clay enameled by X-ray fluorescence technique in Total reflection and by Scanning Electron Microscopy

    International Nuclear Information System (INIS)

    Zarazua O, G.; Carapia M, L.

    2000-01-01

    This work has the objective of determining lead free in the glazed commercial stewing pans using the X-ray fluorescence technique in Total reflection (FRX) and the observation and semiquantitative determination of lead by Analytical Scanning Electron Microscopy (ASEM). (Author)

  2. Development of off-line layer chromatographic and total reflection X-ray fluorescence spectrometric methods for arsenic speciation

    Energy Technology Data Exchange (ETDEWEB)

    Mihucz, Victor G. [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); Moricz, Agnes M. [L. Eoetvoes University, Department of Chemical Technology and Environmental Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Kroepfl, Krisztina [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Szikora, Szilvia [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Tatar, Eniko [Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Parra, Lue Meru Marco [Universidad Centro-occidental Lisandro Alvarado, Decanato de Agronomia, Departamento de Quimica y Suelos Unidad de Analisis Instrumental, Apartado Postal 4076, Cabudare 3023 (Venezuela); Zaray, Gyula [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary) and Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary) and L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary)]. E-mail: zaray@ludens.elte.hu

    2006-11-15

    Rapid and low cost off-line thin layer chromatography-total reflection X-ray fluorescence spectrometry and overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods have been developed for separation of 25 ng of each As(III), As(V), monomethyl arsonic acid and dimethylarsinic acid applying a PEI cellulose stationary phase on plastic sheets and a mixture of acetone/acetic acid/water = 2:1:1 (v/v/v) as eluent system. The type of eluent systems, the amounts (25-1000 ng) of As species applied to PEI cellulose plates, injection volume, development distance, and flow rate (in case of overpressured thin layer chromatography) were taken into consideration for the development of the chromatographic separation. Moreover, a microdigestion method employing nitric acid for the As spots containing PEI cellulose scratched from the developed plates divided into segments was developed for the subsequent total reflection X-ray fluorescence spectrometry analysis. The method was applied for analysis of root extracts of cucumber plants grown in As(III) containing modified Hoagland nutrient solution. Both As(III) and As(V) were detected by applying the proposed thin layer chromatography/overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods.

  3. Development of off-line layer chromatographic and total reflection X-ray fluorescence spectrometric methods for arsenic speciation

    International Nuclear Information System (INIS)

    Mihucz, Victor G.; Moricz, Agnes M.; Kroepfl, Krisztina; Szikora, Szilvia; Tatar, Eniko; Parra, Lue Meru Marco; Zaray, Gyula

    2006-01-01

    Rapid and low cost off-line thin layer chromatography-total reflection X-ray fluorescence spectrometry and overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods have been developed for separation of 25 ng of each As(III), As(V), monomethyl arsonic acid and dimethylarsinic acid applying a PEI cellulose stationary phase on plastic sheets and a mixture of acetone/acetic acid/water = 2:1:1 (v/v/v) as eluent system. The type of eluent systems, the amounts (25-1000 ng) of As species applied to PEI cellulose plates, injection volume, development distance, and flow rate (in case of overpressured thin layer chromatography) were taken into consideration for the development of the chromatographic separation. Moreover, a microdigestion method employing nitric acid for the As spots containing PEI cellulose scratched from the developed plates divided into segments was developed for the subsequent total reflection X-ray fluorescence spectrometry analysis. The method was applied for analysis of root extracts of cucumber plants grown in As(III) containing modified Hoagland nutrient solution. Both As(III) and As(V) were detected by applying the proposed thin layer chromatography/overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods

  4. Censoring: a new approach for detection limits in total-reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Pajek, M.; Kubala-Kukus, A.; Braziewicz, J.

    2004-01-01

    It is shown that the detection limits in the total-reflection X-ray fluorescence (TXRF), which restrict quantification of very low concentrations of trace elements in the samples, can be accounted for using the statistical concept of censoring. We demonstrate that the incomplete TXRF measurements containing the so-called 'nondetects', i.e. the non-measured concentrations falling below the detection limits and represented by the estimated detection limit values, can be viewed as the left random-censored data, which can be further analyzed using the Kaplan-Meier (KM) method correcting for nondetects. Within this approach, which uses the Kaplan-Meier product-limit estimator to obtain the cumulative distribution function corrected for the nondetects, the mean value and median of the detection limit censored concentrations can be estimated in a non-parametric way. The Monte Carlo simulations performed show that the Kaplan-Meier approach yields highly accurate estimates for the mean and median concentrations, being within a few percent with respect to the simulated, uncensored data. This means that the uncertainties of KM estimated mean value and median are limited in fact only by the number of studied samples and not by the applied correction procedure for nondetects itself. On the other hand, it is observed that, in case when the concentration of a given element is not measured in all the samples, simple approaches to estimate a mean concentration value from the data yield erroneous, systematically biased results. The discussed random-left censoring approach was applied to analyze the TXRF detection-limit-censored concentration measurements of trace elements in biomedical samples. We emphasize that the Kaplan-Meier approach allows one to estimate the mean concentrations being substantially below the mean level of detection limits. Consequently, this approach gives a new access to lower the effective detection limits for TXRF method, which is of prime interest for

  5. Characterization of urban air pollution by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Schmeling, Martina

    2004-01-01

    Besides photochemical smog, particulate air pollution is a constantly growing problem in urban areas. The particulate matter present in pollution events contains often toxic or health impacting elements and is responsible for low visibility, might be triggering respiratory diseases like asthma, and can play an important role in formation or duration of smog events. To characterize particulate pollution in two different cities, samples were taken during intensive field campaigns in Chicago, IL, in 2002 and Phoenix, AZ, in 2001. Both cities experience regularly photochemical smog events as well as particulate pollution, but show very different meteorological and topographical conditions. Therefore it is expected that the particulate composition varies significantly, providing information about different pollution forms. Sampling took place in both cases at elevated locations and had a temporal resolution of 1.5 h and 1 h, respectively. The samples were analyzed by total reflection X-ray fluorescence after digestion of the filter matrix. As expected the elemental composition of particulate matter varied between both cities substantially with Phoenix showing a higher abundance of crustal elements, and Chicago enrichment in anthropogenically produced ones. In both cities diurnal patterns were found, exerting maxima in the morning and minima in the early afternoon. The diurnal pattern was much more regularly and also more strongly pronounced in Phoenix. Phoenix's valley location permits for a more stable nocturnal boundary layer to build up during the night thus trapping particulates efficiently during this time, until mixing occurs in the early morning hours and the residual layer lifts. In Chicago, the diurnal variation was less extreme, but another pattern determines the situation with the lake breeze. The lake breeze corresponds to a shift in wind direction towards the east, i.e. from Lake Michigan during the late morning. It was found that certain elemental species

  6. Recent results of synchrotron radiation induced total reflection X-ray fluorescence analysis at HASYLAB, beamline L

    Energy Technology Data Exchange (ETDEWEB)

    Streli, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, A-1020 Vienna (Austria)]. E-mail: streli@ati.ac.at; Pepponi, G. [ITC-irst, Povo (Italy); Wobrauschek, P. [Atominstitut, Vienna University of Technology, Stadionallee 2, A-1020 Vienna (Austria); Jokubonis, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, A-1020 Vienna (Austria); Falkenberg, G. [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, D-22603 Hamburg (Germany); Zaray, G. [Institute of Inorganic and Applied Chemistry, 3 EOTVOS Univ, Budapest (Hungary); Broekaert, J. [Institute of Anorganic and Applied Chemistry, University Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Fittschen, U. [Institute of Anorganic and Applied Chemistry, University Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Peschel, B. [Institute of Anorganic and Applied Chemistry, University Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany)

    2006-11-15

    At the Hamburger Synchrotronstrahlungslabor (HASYLAB), Beamline L, a vacuum chamber for synchrotron radiation-induced total reflection X-ray fluorescence analysis, is now available which can easily be installed using the adjustment components for microanalysis present at this beamline. The detector is now in the final version of a Vortex silicon drift detector with 50-mm{sup 2} active area from Radiant Detector Technologies. With the Ni/C multilayer monochromator set to 17 keV extrapolated detection limits of 8 fg were obtained using the 50-mm{sup 2} silicon drift detector with 1000 s live time on a sample containing 100 pg of Ni. Various applications are presented, especially of samples which are available in very small amounts: As synchrotron radiation-induced total reflection X-ray fluorescence analysis is much more sensitive than tube-excited total reflection X-ray fluorescence analysis, the sampling time of aerosol samples can be diminished, resulting in a more precise time resolution of atmospheric events. Aerosols, directly sampled on Si reflectors in an impactor were investigated. A further application was the determination of contamination elements in a slurry of high-purity Al{sub 2}O{sub 3}. No digestion is required; the sample is pipetted and dried before analysis. A comparison with laboratory total reflection X-ray fluorescence analysis showed the higher sensitivity of synchrotron radiation-induced total reflection X-ray fluorescence analysis, more contamination elements could be detected. Using the Si-111 crystal monochromator also available at beamline L, XANES measurements to determine the chemical state were performed. This is only possible with lower sensitivity as the flux transmitted by the crystal monochromator is about a factor of 100 lower than that transmitted by the multilayer monochromator. Preliminary results of X-ray absorption near-edge structure measurements for As in xylem sap from cucumber plants fed with As(III) and As(V) are

  7. Recent results of synchrotron radiation induced total reflection X-ray fluorescence analysis at HASYLAB, beamline L

    International Nuclear Information System (INIS)

    Streli, C.; Pepponi, G.; Wobrauschek, P.; Jokubonis, C.; Falkenberg, G.; Zaray, G.; Broekaert, J.; Fittschen, U.; Peschel, B.

    2006-01-01

    At the Hamburger Synchrotronstrahlungslabor (HASYLAB), Beamline L, a vacuum chamber for synchrotron radiation-induced total reflection X-ray fluorescence analysis, is now available which can easily be installed using the adjustment components for microanalysis present at this beamline. The detector is now in the final version of a Vortex silicon drift detector with 50-mm 2 active area from Radiant Detector Technologies. With the Ni/C multilayer monochromator set to 17 keV extrapolated detection limits of 8 fg were obtained using the 50-mm 2 silicon drift detector with 1000 s live time on a sample containing 100 pg of Ni. Various applications are presented, especially of samples which are available in very small amounts: As synchrotron radiation-induced total reflection X-ray fluorescence analysis is much more sensitive than tube-excited total reflection X-ray fluorescence analysis, the sampling time of aerosol samples can be diminished, resulting in a more precise time resolution of atmospheric events. Aerosols, directly sampled on Si reflectors in an impactor were investigated. A further application was the determination of contamination elements in a slurry of high-purity Al 2 O 3 . No digestion is required; the sample is pipetted and dried before analysis. A comparison with laboratory total reflection X-ray fluorescence analysis showed the higher sensitivity of synchrotron radiation-induced total reflection X-ray fluorescence analysis, more contamination elements could be detected. Using the Si-111 crystal monochromator also available at beamline L, XANES measurements to determine the chemical state were performed. This is only possible with lower sensitivity as the flux transmitted by the crystal monochromator is about a factor of 100 lower than that transmitted by the multilayer monochromator. Preliminary results of X-ray absorption near-edge structure measurements for As in xylem sap from cucumber plants fed with As(III) and As(V) are reported. Detection

  8. 1. Latin American Workshop on Total Reflection X-Ray Fluorescence (TXRF) and its Applications: TARABANA 99. Programme and Abstracts

    International Nuclear Information System (INIS)

    Vegas C, Fredy; Greaves N, Eduardo; Marco P, Lue-Meru

    1999-01-01

    It concerns about the advances in Total Reflection X-Ray Fluorescence (TXRF) instrumentation; structure, characteristic and potential of TXRF equipment used for chemical multielemental survey; TXRF: an approach to nano analysis; microanalytical investigation of environmental samples by TXRF spectrometry; TXRF of low Z elements; assessment of serum selenium levels in 2 month old sucking calves using TXRF: A powerful method to investigate the elemental composition of spheroids; environmental applications of TXRF; use of modifiers for the elimination in situ of chlorides in the analysis of TXRF; experimental methodology and analysis spectra for the determination of mercury by means of TXRF using amalgamation with gold; multielemental analysis of human amniotic fluid by use of Total Reflection X-Ray Fluorescence and rutherford forward scattering; determination of metal in samples of handmade penca; determination of oligo elements, platinum and relationship Zn/Cu in samples of blood serum and urine in oncological pediatric patient [es

  9. Determination of solid surface composition by the X-ray fluorescence method under total external reflection with angular scanning

    International Nuclear Information System (INIS)

    Krasnolutskij, V.P.

    2000-01-01

    Possibilities of determination of composition of surface layers by X-ray fluorescence analysis under total reflection of incident radiation with angular scanning of a target are investigated. For the case of the GaAs target it is shown that the sensibility of this method is sufficient for a control of element composition in layer of thickness 1 nm. A simple method for solution of inverse task of analysis of a two component medium is considered [ru

  10. Pigment particles analysis with a total reflection X-ray fluorescence spectrometer: study of influence of instrumental parameters

    Energy Technology Data Exchange (ETDEWEB)

    Coccato, Alessia; Vandenabeele, Peter [Ghent University, Department of Archaeology, Ghent (Belgium); Vekemans, Bart; Vincze, Laszlo; Moens, Luc [Ghent University, Department of Analytical Chemistry, Ghent (Belgium)

    2016-12-15

    Total reflection X-ray fluorescence (TXRF) analysis is an excellent tool to determine major, minor and trace elements in minuscule amounts of samples, making this technique very suitable for pigment analysis. Collecting minuscule amounts of pigment material from precious works of art by means of a cotton swab is a well-accepted sampling method, but poses specific challenges when TXRF is to be used for the characterization of the unknown material. (orig.)

  11. Total reflection X-ray fluorescence analysis of trace-elements in candies marketed in Mexico

    International Nuclear Information System (INIS)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2010-01-01

    Trace metals concentrations in food are significant for nutrition, due either to their nature or toxicity. Sweets, including chewing gum and candies, are not exactly a food, but they usually are unwearied consumed by children, the most vulnerable age-group to any kind of metal contamination in the food chain. The presence of relatively high concentrations of heavy metals such as Lead elicits concern since children are highly susceptible to heavy metals poisoning. Trace-metals concentrations were determined for six different flavors of a Mexican candy by means of Total X-ray Fluorescence Spectrometry. Triplicate samples of the various candy's flavours (strawberry, pineapple, lemon, blackberry, orange and chilli) were digested in 8 mL of a mix of supra-pure HNO 3 and H 2 O 2 (6 mL: 2 mL) in a microwave oven MARS-X. Results show the presence of essential and toxic elements such as Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, and Pb. All metal concentrations were higher and significantly different (α = 0.05) in chilli candy, compared to other candy flavours. Lead concentration fluctuated in the range of 0.102 to 0.342 μg g -1 . A discussion about risk consumption and concentration allowed by Mexican and International Norms is made. As a part of the Quality Control Program, a NIST standard of 'Citrus Leaves' and a blank were treated in the same way.

  12. Total reflection X-ray fluorescence analysis of trace-elements in candies marketed in Mexico

    Science.gov (United States)

    Martinez, T.; Lartigue, J.; Zarazua, G.; Avila-Perez, P.; Navarrete, M.; Tejeda, S.

    2010-06-01

    Trace metals concentrations in food are significant for nutrition, due either to their nature or toxicity. Sweets, including chewing gum and candies, are not exactly a food, but they usually are unwearied consumed by children, the most vulnerable age-group to any kind of metal contamination in the food chain. The presence of relatively high concentrations of heavy metals such as Lead elicits concern since children are highly susceptible to heavy metals poisoning. Trace-metals concentrations were determined for six different flavors of a Mexican candy by means of Total X-ray Fluorescence Spectrometry. Triplicate samples of the various candy's flavours (strawberry, pineapple, lemon, blackberry, orange and chilli) were digested in 8 mL of a mix of supra-pure HNO 3 and H 2O 2 (6 mL: 2 mL) in a microwave oven MARS-X. Results show the presence of essential and toxic elements such as Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, and Pb. All metal concentrations were higher and significantly different ( α = 0.05) in chilli candy, compared to other candy flavours. Lead concentration fluctuated in the range of 0.102 to 0.342 μg g - 1 . A discussion about risk consumption and concentration allowed by Mexican and International Norms is made. As a part of the Quality Control Program, a NIST standard of "Citrus Leaves" and a blank were treated in the same way.

  13. Application of a portable total reflection x-ray fluorescence spectrometer to a trace elemental analysis of wines

    International Nuclear Information System (INIS)

    Kunimura, Shinsuke; Kawai, Jun

    2009-01-01

    A portable total reflection X-ray fluorescence (TXRF) spectrometer has been applied to a trace elemental analysis of wines. Sulfur, K, Mn, Fe, and Rb were detected. These five elements were quantified by using 1 ppm of Co as an internal standard. The quantified concentrations ranged from sub-ppm to several hundred ppm. Because of organic substances in wines, the scattering of the incident X-rays from the dry residues of wines becomes strong. Therefore, a high spectral background appears in TXRF spectra of wines. Because of this background, relative standard deviations of the quantified concentrations were from 4 to 28%. Although the high spectral background appeared in the TXRF spectra of the wines, a detection limit down to several tens of ppb was achieved. The present portable spectrometer can be applied to screening for trace elements in wines before an accurate and precise analysis using a large elemental analyzer. (author)

  14. Total reflection X-ray fluorescence analysis of trace-elements in candies marketed in Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, T., E-mail: tmc@servidor.unam.m [Facultad de Quimica, Departamento de Quimica Inorganica y Nuclear. Universidad Nacional Autonoma de Mexico, Mexico D.F. 04510 (Mexico); Lartigue, J. [Facultad de Quimica, Departamento de Quimica Inorganica y Nuclear. Universidad Nacional Autonoma de Mexico, Mexico, D.F. 04510 (Mexico); Zarazua, G.; Avila-Perez, P. [National Institute of Nuclear Research. Ocoyoacac, Edo. de Mexico, 05045 (Mexico); Navarrete, M. [Facultad de Quimica, Departamento de Quimica Inorganica y Nuclear. Universidad Nacional Autonoma de Mexico, Mexico, D.F. 04510 (Mexico); Tejeda, S. [National Institute of Nuclear Research. Ocoyoacac, Edo. de Mexico, 05045 (Mexico)

    2010-06-15

    Trace metals concentrations in food are significant for nutrition, due either to their nature or toxicity. Sweets, including chewing gum and candies, are not exactly a food, but they usually are unwearied consumed by children, the most vulnerable age-group to any kind of metal contamination in the food chain. The presence of relatively high concentrations of heavy metals such as Lead elicits concern since children are highly susceptible to heavy metals poisoning. Trace-metals concentrations were determined for six different flavors of a Mexican candy by means of Total X-ray Fluorescence Spectrometry. Triplicate samples of the various candy's flavours (strawberry, pineapple, lemon, blackberry, orange and chilli) were digested in 8 mL of a mix of supra-pure HNO{sub 3} and H{sub 2}O{sub 2} (6 mL: 2 mL) in a microwave oven MARS-X. Results show the presence of essential and toxic elements such as Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr, and Pb. All metal concentrations were higher and significantly different ({alpha} = 0.05) in chilli candy, compared to other candy flavours. Lead concentration fluctuated in the range of 0.102 to 0.342 {mu}g g{sup -1}. A discussion about risk consumption and concentration allowed by Mexican and International Norms is made. As a part of the Quality Control Program, a NIST standard of 'Citrus Leaves' and a blank were treated in the same way.

  15. Modelling of a total reflection X-ray fluorescence (TXRF) system ...

    African Journals Online (AJOL)

    The simulation of the different stages involved in x-ray fluorescence emissions was carried out by writing a suite of computer programs using FORTRAN programming language. These computer simulated XRF stages were then integrated together to generate a general robust model which was run with the digital visual ...

  16. Analytical characterization of artists' pigments used in old and modern paintings by total-reflection x-ray fluorescence

    International Nuclear Information System (INIS)

    Klockenkaemper, R.; Bohlen, A. von; Moens, L.; Devos, W.

    1993-01-01

    The analytical characterization of artists' pigments is a most helpful tool for art history, conservation and restoration of paintings. A very gentle method of ultra-microsampling was developed that is especially applicable to paintings under restoration. It provides a sample mass of about 1 μg and is virtually non-destructive. This minute amount is sufficient for total-reflection X-ray fluorescence (TXRF) to determine most of those elements building inorganic pigments. The convenient and fast method was applied to oil paintings. Various pigments were identified and their mixing proportion was determined even quantitatively. (author)

  17. Trace elemental analysis of leaching solutions of hijiki seaweeds by a portable total reflection X-ray fluorescence spectrometer

    International Nuclear Information System (INIS)

    Liu, Ying; Imashuku, Susumu; Kawai, Jun

    2014-01-01

    A portable total reflection X-ray fluorescence spectrometer (TXRF) was used to analyze leaching solutions of hijiki seaweeds. S, Cl, K, Ca, Ti, Fe, Ni, As and Br were detected in the solutions. Arsenic quantification results were compared to those from ICP-AES. The TXRF quantification results of arsenic were not significantly different from those of ICP-AES, as two-way analysis of variance (ANOVA) method was applied to the significance test. This kind of small and high sensitive TXRF spectrometer can be used in food quality and environmental pollution investigation. (author)

  18. Elemental concentration in normal skin and fibroepithelial polip lesions by synchrotron radiation total reflection X-ray fluorescence technique

    International Nuclear Information System (INIS)

    Soares, Julio C.A.C.R.; Canellas, Catarine G.L.; Lopes, Ricardo T.; Anjos, Marcelino J.

    2011-01-01

    In this work, the concentrations of trace elements were measured in acrochordon, a skin lesion also known as skin tag or fibroepithelial polyp, as well as in normal skin from the same patient. The samples were analysed by Synchrotron Radiation Total Reflection X- ray Fluorescence (SRTXRF) in the Synchrotron Light National Laboratory (LNLS) in Campinas/Sao Paulo-Brazil. The collection of lesion and healthy skin samples, including papillary dermis and epidermis, has involved 17 patients. It was evaluated the presence of P, S, Cl, K, Ca, Cr, Mn, Fe, Cu, Zn, Br and Rb in the paired samples, which were compared, and significant differences were found in some of them. (author)

  19. A method for thickness determination of thin films of amalgamable metals by total-reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Bennun, L.; Greaves, E.D.; Barros, H.; Diaz-Valdes, J.

    2009-01-01

    A method for thickness determination of thin amalgamable metallic films by total-reflection X-ray fluorescence (TXRF) is presented. The peak's intensity in TXRF spectra are directly related to the surface density of the sample, i.e. to its thickness in a homogeneous film. Performing a traditional TXRF analysis on a thin film of an amalgamated metal, and determining the relative peak intensity of a specific metal line, the layer thickness can be precisely obtained. In the case of gold thickness determination, mercury and gold peaks overlap, hence we have developed a general data processing scheme to achieve the most precise results.

  20. Total reflection X-ray fluorescence analysis of river waters in its stream across the city of Cordoba, in Argentina

    International Nuclear Information System (INIS)

    Valentinuzzi, M.C.; Sanchez, H.J.; Abraham, J.

    2006-01-01

    The aim of this work was to analyze the composition of river waters and to study their quality by detecting possible contaminants. The samples were taken at 32 points of the Suquia River in its stream across the city of Cordoba (in the Province of Cordoba, Argentina). The samples were analyzed with total reflection X-ray fluorescence (TXRF) using beam guides. Beam guides made of two Si plate reflectors were used as sample carriers and to guide the X-ray photons to the sample; the measurements were taken using the characteristic configuration that ensures the best excitation and detection conditions (in TXRF). The analyses were carried out by preconcentration of the water samples and by adding an internal standard (Gallium); small amounts of samples (30 μl) were deposited on the Si reflector plate and they were then analyzed in the total reflection regime. Spectra were analyzed with standard methods using conventional programs. The results show interesting behaviors of the concentration of trace elements along the river: elements of low atomic number (such as Ca, Cl, S, K) present higher concentrations as compared to high Z elements (such as Fe, Zn, Br, Sr); the concentrations of light elements follow a similar behavior along the stream, the same situation is observed in the set of elements with high atomic number. Some samples present high concentrations in certain elements indicating possible sources of contamination

  1. Energy dispersive X-ray fluorescence analysis with multiple total reflection

    International Nuclear Information System (INIS)

    Freitag, K.

    1985-01-01

    The development of a total reflection XRF analyzer and the performance data of this instrument are described. The drastic reduction of the scattered radiation is the outstanding property of the method. Detection limits of elements and matrix effects are discussed. The competition with other methods of analysis has proven its advantages in a wide range. In addition to its multi-element features down to the picogram level, particularly its universal calibration function has turned out to be a great help in the analytical practice. (orig./RB)

  2. On revealing the vertical structure of nanoparticle films with elemental resolution: A total external reflection X-ray standing waves study

    Energy Technology Data Exchange (ETDEWEB)

    Zargham, Ardalan, E-mail: zargham@ifp.uni-bremen.d [Institute of Solid State Physics, University of Bremen, Otto-Hahn-Allee 1, 28359 Bremen (Germany); Schmidt, Thomas; Flege, Jan Ingo; Sauerbrey, Marc; Hildebrand, Radowan [Institute of Solid State Physics, University of Bremen, Otto-Hahn-Allee 1, 28359 Bremen (Germany); Roehe, Sarah; Baeumer, Marcus [Applied and Physical Chemistry, University of Bremen, Leobener Str. 2, 28359, Bremen (Germany); Falta, Jens [Institute of Solid State Physics, University of Bremen, Otto-Hahn-Allee 1, 28359 Bremen (Germany)

    2010-02-15

    We present a promising combination of methods to precisely determine the morphology of nanostructures, drawing on the example of monodisperse CoPt{sub 3} nanoparticle films deposited by spin coating and dip coating techniques on functionalized Au substrates. Ex-situ X-ray standing waves in total external reflection combined with X-ray reflectivity measurements were employed to determine element-specific atomic-density distributions in vertical direction.

  3. Characterization of ancient coins with the use of total reflection x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Ostachowicz, B.; Holynska, B.; Ostachowicz, J.; Haczewska, B.

    2000-01-01

    In this work the composition of silver coins from XI-XII centuries and a metal gorget from XVIII century have been studied. The beginnings of denarii (Sachsenpfennige) coinage might be linked with Saxony, whereas the end period of the production of those coins i.e. the last quarter of the XI th and beginning of the XII th centuries is connected also with Polish mints. The studied coins bearing the chivalric cross upon the reverse were minted by Wladyslaw Herman a Polish prince and his palatine Sieciech. Some of the coins were original ones, some other were forged, however the provenance of both types of coins was probably the same. The forged coins contained copper core covered with silver alloy. The TXRF module with molybdenum x-ray tube operated at 55 kV and 40 mA has been used for analysis of both types of coins. A quartz reflector was rubbed against a coin and then analyzed. Several metals were found and determined in the coins namely: zinc, copper, iron, lead and also trace concentrations of gold and mercury. A small piece of silver coin was also dissolved in nitric acid and a solution was analyzed by TXRF. The results showed good agreement with the data obtained by rubbing a coin. The gorget was made of gilded copper and decorated by paintings presenting a Holy Mary and Jesus Christ. The metal parts of the gorget was rubbed against quartz reflectors and analyzed. The concentration of major and minor elements in metal gives an important information for historian of art about technology of production and decoration of gorgets. The traces of mercury were found in the golden layer. This suggested that making Au-Hg amalgam followed by heating was used for covering a copper gorget with the layer of gold. (author)

  4. Determination of mercury in seawater by total reflection x-ray fluorescence spectrometry after an electrochemical preconcentration method

    International Nuclear Information System (INIS)

    Ritschel, A.; Chinea Cano, E.; Wobrauschek, P.; Kuntner, C.; Durakbasa, M.N.

    2000-01-01

    A new combined method of electrodeposition of trace elements on metallic plates with subsequent total-reflection x-ray fluorescence spectrometry (TXRF) is proposed for the determination of trace metals in natural waters. The elements of interest are electroplated on highly polished niobium discs which are used as sample carriers for the TXRF measurement. The electrochemical preconcentration is performed in a flow cell under a controlled working electrode potential. The preconcentration step involves only very little manipulation which minimizes the risk of contamination of the sample. The method was investigated by analyzing inorganic mercury in sea water. A detection limit of 7 ngl -1 could be achieved for mercury in a 40 ml sea water sample. (author)

  5. Fish samples as bioindicator of environmental quality: synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    International Nuclear Information System (INIS)

    Vives, Ana Elisa Sirito de; Moreira, Silvana; Brienza, Sandra Maria Boscolo; Zucchi, Orgheda Luiza Araujo Domingues; Nascimento Filho, Virgilio Franco do Centro de Energia Nuclear na Agricultura , Piracicaba, SP; Brazil)

    2005-01-01

    In this study fish were used as bioindicators of environmental contamination. The species were collected in Piracicaba River, Sao Paulo state, Brazil and the toxic elements concentrations were determined in muscle tissue and viscus (liver, intestine and stomach) by Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF). Were determined the elements Ti, Cr, Mn, Fe, Ni, Cu, Zn and Ba. The results were compared with values established by Brazilian Legislation for general food. The elements concentrations evidenced potential risk to human health and environmental quality alteration of the studied area. The measurements were realized at the 'Laboratorio Nacional de Luz Sincrotron' (LNLS) located in Campinas, Sao Paulo State, Brazil. (author)

  6. Determination of copper, iron and zinc in spirituous beverages by total reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Capote, T.; Marcó, L. M.; Alvarado, J.; Greaves, E. D.

    1999-10-01

    The concentration of copper in traditional homemade alcoholic distillates produced in Venezuela (Cocuy de Penca) were determined by total reflection X-ray fluorescence (TXRF) using vanadium as internal standard. The results were compared to those obtained by flame atomic absorption spectrometry (FAAS). Three preparative methods of addition of vanadium were compared: classical internal standard addition, 'layer on layer' internal standard addition and in situ addition of internal standard. The TXRF procedures were accurate and the precision was comparable to that obtained by the FAAS technique. Copper levels were above the maximum allowed limits for similar beverages. Zinc and iron in commercial and homemade distilled beverages were also analyzed by TXRF with in situ addition of internal standard demonstrating the usefulness of this technique for trace metal determination in distillates.

  7. Fish samples as bioindicator of environmental quality: synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Brienza, Sandra Maria Boscolo [Universidade Metodista de Piracicaba (UNIMEP), SP (Brazil). Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)]. E-mail: virgilio@cena.usp.br

    2005-07-01

    In this study fish were used as bioindicators of environmental contamination. The species were collected in Piracicaba River, Sao Paulo state, Brazil and the toxic elements concentrations were determined in muscle tissue and viscus (liver, intestine and stomach) by Synchrotron Radiation Total Reflection X-Ray Fluorescence Analysis (SR-TXRF). Were determined the elements Ti, Cr, Mn, Fe, Ni, Cu, Zn and Ba. The results were compared with values established by Brazilian Legislation for general food. The elements concentrations evidenced potential risk to human health and environmental quality alteration of the studied area. The measurements were realized at the 'Laboratorio Nacional de Luz Sincrotron' (LNLS) located in Campinas, Sao Paulo State, Brazil. (author)

  8. Trajectory method in the theory of Laue diffraction of X rays in crystals: II. Effect of total reflection at bending deformation

    International Nuclear Information System (INIS)

    Kohn, V. G.

    2008-01-01

    The effect of total reflection (switching) of a spherical X-ray wave in the case of Laue diffraction in a crystal with bending deformation is analyzed by the trajectory method. Qualitative analytical description and computation of the spatial structure of the reflected beam for large and small distances between the spherical-wave source and the crystal are performed. The mechanism of much more efficient reflection of an X-ray beam by a deformed crystal in comparison with a perfect crystal is clearly demonstrated. It is also shown that the trajectory method is very convenient for description of the total reflection phenomenon.

  9. Trajectory method in the theory of Laue diffraction of X rays in crystals: II. Effect of total reflection at bending deformation

    International Nuclear Information System (INIS)

    Kohn, V. G.

    2008-01-01

    The effect of total reflection (switching) of a spherical X-ray wave in the case of Laue diffraction in a crystal with bending deformation is analyzed by the trajectory method. Qualitative analytical description and computation of the spatial structure of the reflected beam for large and small distances between the spherical-wave source and the crystal are performed. The mechanism of much more efficient reflection of an X-ray beam by a deformed crystal in comparison with a perfect crystal is clearly demonstrated. It is also shown that the trajectory method is very convenient for description of the total reflection phenomenon

  10. Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

    International Nuclear Information System (INIS)

    Hoefler, H.; Streli, C.; Wobrauschek, P.; Ovari, M.; Zaray, Gy.

    2006-01-01

    Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm 2 active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors

  11. Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hoefler, H. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria); Streli, C. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria)]. E-mail: streli@ati.ac.at; Wobrauschek, P. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria); Ovari, M. [Eoetvoes University, Institute of Chemistry, H-1117, Budapest, Pazmany P. stny 1/a. (Hungary); Zaray, Gy. [Eoetvoes University, Institute of Chemistry, H-1117, Budapest, Pazmany P. stny 1/a. (Hungary)

    2006-11-15

    Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm{sup 2} active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors.

  12. Elemental concentration analysis in the brain of young and old Wistar rats by total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T.; Anjos, Marcelino J. dos; Carmo, Maria G.T. do; Rocha, Monica S.; Moreira, Silvana; Martinez, Ana M.B.

    2007-01-01

    It is well known that aging is associated with neurobehavioral deficits. The aging process of human brain is characterized by progressive neuronal loss. Furthermore, certain brain areas are more vulnerable to neuronal degeneration than others, reflecting an altered resistance to stress of the tissue itself and/or the lack of adequate immunological defense mechanisms in these regions. About the elemental levels in the brain, it is known that the excess ou deficiency of some elements are toxic for human healthy, being also related to several neurodegenerative diseases. In this way, the main goal of this work was to determine the elemental concentration in the hippocampus of young and old male (n = 10) and female (n = 10) Wistar rats by total reflection X-ray fluorescence spectrometry with synchrotron radiation (SR-TXRF). These measurements were carried out at XRF beam line at Light Synchrotron Brazilian Laboratory, Campinas, Brazil. About the results, we could observe that Al, Fe, Cu, Zn and Br levels were higher in the hippocampus of the old female rats than the young ones. On the other hand, only Cu levels were higher in the hippocampus of the old male rats than the young ones. Therefore, the aging of the hippocampus of the female rats can be characterized by an accumulate for Al, Fe, Cu, Zn and Br. The excess in these elements levels are also associated with several neurodegenerative disorders, such as Alzheimer' disease, Parkinson's disease and Huntington's disease. (author)

  13. Worldwide distribution of Total Reflection X-ray Fluorescence instrumentation and its different fields of application: A survey

    Energy Technology Data Exchange (ETDEWEB)

    Klockenkämper, Reinhold, E-mail: reinhold.klockenkaemper@isas.de; Bohlen, Alex von

    2014-09-01

    A survey was carried out with users and manufacturers of Total Reflection X-ray Fluorescence instrumentation in order to demonstrate the worldwide distribution of TXRF equipment and the different fields of applications. In general, TXRF users come from universities and scientific institutes, from working places at synchrotron beam-lines, or laboratories in semiconductor fabs. TXRF instrumentation is distributed in more than 50 countries on six continents and is applied at about 200 institutes and laboratories. The number of running desktop instruments amounts to nearly 300 units. About 60 beamlines run working places dedicated to TXRF. About 300 floor-mounted instruments are estimated to be used in about 150 fabs of the semiconductor industry. In total, 13 different fields of applications could be registered statistically from three different aspects. - Highlights: • According to the survey world maps show the distribution of TXRF equipment. • Nearly 700 individual units are running actually in 57 countries of 6 continents. • Users work at 200 universities, 60 synchrotron-beamlines, and 150 semiconductor fabs. • 13 fields of applications (e.g. environmental, chemical) are evaluated statistically. • Manufacturers, conference members and authors lead to 3 different pie-charts.

  14. Total reflection X-ray fluorescence as a convenient tool for determination of trace elements in microscale gasoline and diesel

    Science.gov (United States)

    Zhang, Airui; Jin, Axiang; Wang, Hai; Wang, Xiaokang; Zha, Pengfei; Wang, Meiling; Song, Xiaoping; Gao, Sitian

    2018-03-01

    Quantitative determination of trace elements like S, Fe, Cu, Mn and Pb in gasoline and S in diesel is of great importance due to the growing concerns over air pollution, human health and engine failure caused by utilization of gasoline and diesel with these harmful elements. A method of total reflection X-ray fluorescence (TXRF) was developed to measure these harmful trace elements in gasoline and diesel. A variety of factors to affect measurement results, including TXRF parameters, microwave-assisted digestion conditions and internal standard element and its addition, were examined to optimize these experimental procedures. The hydrophobic treatment of the surface of quartz reflectors to support the analyte with neutral silicone solutions could prepare thin films of gasoline and diesel digestion solutions for subsequent TXRF analysis. The proposed method shows good potential and reliability to determine the content of harmful trace elements in gasoline and diesel with high sensitivity and accuracy without drawing different standard calibration curves, and can be easily employed to screen gasoline and diesel in routine quality control and assurance.

  15. Total reflection x-ray fluorescence spectroscopy as a tool for evaluation of iron concentration in ferrofluids and yeast samples

    Energy Technology Data Exchange (ETDEWEB)

    Kulesh, N.A., E-mail: nikita.kulesh@urfu.ru [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Novoselova, I.P. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Immanuel Kant Baltic Federal University, 236041 Kaliningrad (Russian Federation); Safronov, A.P. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Institute of Electrophysics UD RAS, Amundsen 106, 620016 Ekaterinburg (Russian Federation); Beketov, I.V.; Samatov, O.M. [Institute of Electrophysics UD RAS, Amundsen 106, 620016 Ekaterinburg (Russian Federation); Kurlyandskaya, G.V. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); University of the Basque Country UPV-EHU, 48940 Leioa (Spain); Morozova, M. [Ural Federal University, Mira 19, 620002 Ekaterinburg (Russian Federation); Denisova, T.P. [Irkutsk State University, Karl Marks 1, 664003 Irkutsk (Russian Federation)

    2016-10-01

    In this study, total reflection x-ray fluorescent (TXRF) spectrometry was applied for the evaluation of iron concentration in ferrofluids and biological samples containing iron oxide magnetic nanoparticles obtained by the laser target evaporation technique. Suspensions of maghemite nanoparticles of different concentrations were used to estimate the limitation of the method for the evaluation of nanoparticle concentration in the range of 1–5000 ppm in absence of organic matrix. Samples of single-cell yeasts grown in the nutrient media containing maghemite nanoparticles were used to study the nanoparticle absorption mechanism. The obtained results were analyzed in terms of applicability of TXRF for quantitative analysis in a wide range of iron oxide nanoparticle concentrations for biological samples and ferrofluids with a simple established protocol of specimen preparation. - Highlights: • Ferrofluids and yeasts samples were analysed by TXRF spectroscopy. • Simple protocol for iron quantification by means of TXRF was proposed. • Results were combined with magnetic, structural, and morphological characterization. • Preliminary conclusion on nanoparticles uptake mechanism was made.

  16. Inorganic pigment study of the San Pedro Gonzalez Telmo Sibyls using total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Vazquez, Cristina, E-mail: vazquez@cnea.gov.a [Universidad de Buenos Aires, Facultad de Ingenieria, Paseo Colon 850. C1063ACU, Buenos Aires (Argentina); Comision Nacional de Energia Atomica, Gerencia Quimica, Av. Gral Paz 1499, B1650KNA, San Martin (Argentina); Custo, Graciela, E-mail: custo@cnea.gov.a [Comision Nacional de Energia Atomica, Gerencia Quimica, Av. Gral Paz 1499, B1650KNA, San Martin (Argentina); Barrio, Nestor, E-mail: nbarrio@unsam.edu.a [CEIRCAB-TAREA, Universidad Nacional de San Martin (UNSAM), Escuela de Humanidades, Campus Miguelete, 25 de Mayo y Francia, B1650KNA, San Martin (Argentina); Burucua, Jose, E-mail: gburucua@unsam.edu.a [CEIRCAB-TAREA, Universidad Nacional de San Martin (UNSAM), Escuela de Humanidades, Campus Miguelete, 25 de Mayo y Francia, B1650KNA, San Martin (Argentina); Boeykens, Susana [Universidad de Buenos Aires, Facultad de Ingenieria, Paseo Colon 850. C1063ACU, Buenos Aires (Argentina); Marte, Fernando, E-mail: fmarte@unsam.edu.a [CEIRCAB-TAREA, Universidad Nacional de San Martin (UNSAM), Escuela de Humanidades, Campus Miguelete, 25 de Mayo y Francia, B1650KNA, San Martin (Argentina)

    2010-09-15

    This article describes the study carried out on a series of oil paintings on canvas from the eighteenth century that were restored at Centro de Produccion e Investigacion en Restauracion y Conservacion Artistica y Bibliografica - Tarea (CEIRCAB-Tarea), Buenos Aires, Argentina: the San Pedro Gonzalez Telmo Sibyls. Experimental study was undertaken to identify inorganic pigments and the technique used in their confection; and, in this way, try to add information about their local origin. Therefore special emphasis was put to infer technologies used in the manufacturing of these paintings. Elemental analysis was performed by total reflection X-ray fluorescence spectrometry (TXRF) and complemented by optical and polarized light microscopy. Microsampling was carefully done over areas of the paintings which were damaged and where a small additional loss will not be noticed. This investigation has shown that a variety of pigments were used, namely earth pigments (red and yellow ochres), white lead, vermilion, etc., and they were used either pure or in mixtures. This characterization helped conservators in their decisions regarding a better understanding of the deterioration processes. In addition, this research about the material composition allowed the art historians and restorers the possibility to obtain information about where, when or by whom The San Pedro Gonzalez Telmo Sibyls may have been painted.

  17. Total reflection X-ray spectroscopy as a rapid analytical method for uranium determination in drainage water

    International Nuclear Information System (INIS)

    Matsuyama, Tsugufumi; Sakai, Yasuhiro; Izumoto, Yukie; Imaseki, Hitoshi; Hamano, Tsuyoshi; Yoshii, Hiroshi

    2017-01-01

    Uranium concentrations in drainage water are typically determined by α-spectrometry. However, due to the low specific radioactivity of uranium, the evaporation of large volumes of drainage water, followed by several hours of measurements, is required. Thus, the development of a rapid and simple detection method for uranium in drainage water would enhance the operation efficiency of radiation control workers. We herein propose a novel methodology based on total reflection X-ray fluorescence (TXRF) for the measurement of uranium in contaminated water. TXRF is a particularly desirable method for the rapid and simple evaluation of uranium in contaminated water, as chemical pretreatment of the sample solution is not necessary, measurement times are typically several seconds, and the required sample volume is low. We herein employed sample solutions containing several different concentrations of uranyl acetate with yttrium as an internal standard. The solutions were placed onto sample holders, and were dried prior to TXRF measurements. The relative intensity, otherwise defined as the net intensity ratio of the Lα peak of uranium to the Kα peak of yttrium, was directly proportional to the uranium concentration. Using this method, a TXRF detection limit for uranium in contaminated water of 0.30 μg/g was achieved. (author)

  18. Trace metal determinations by total-reflection x-ray fluorescence analysis in the open Atlantic Ocean

    International Nuclear Information System (INIS)

    Schmidt, D.; Gerwinski, W.; Radke, I.

    1993-01-01

    The Intergovernmental Oceanographic Commission (IOC), as a major component of its programme ''Global Investigation of Pollution in the Marine Environment'' (GIPME), maintains a long-standing project on ''Open Ocean Baseline Studies of Trace Contaminants''. Initially, the Atlantic Ocean and trace metals were selected. Four deep-water stations in the Cape Basin, Angola Basin, Cape Verde Abyssal Plain and Seine Abyssal Plain were regularly sampled for at least 36 depths. Additional samples were taken between stations. Samples were distributed to participants and a similar number of additional laboratories. As a central part of our own contribution to the project, we determined the trace heavy metals manganese, nickel, copper, zinc and lead and the lighter selenium by total-reflection X-ray fluorescence analysis. For the TXRF, the pre-enrichment of the trace metals and the separation from the salt matrix were performed by complexation with sodium dibenzyldithiocarbamate and reverse-phase chromatography. Generally, very low levels of trace elements were found in filtered and unfiltered water samples from these remote areas of the open Atlantic Ocean. Typical examples of the distributions of trace metal concentrations on depth profiles from the four deep-water stations as well as intercomparisons between the stations are presented. (author)

  19. Determination of arsenic in water samples by Total Reflection X-Ray Fluorescence using pre-concentration with alumina

    Energy Technology Data Exchange (ETDEWEB)

    Barros, Haydn [Laboratorio de Fisica Nuclear, Dpto. De Fisica, Universidad Simon Bolivar, Sartenejas, Baruta (Venezuela, Bolivarian Republic of); Marco Parra, Lue-Meru, E-mail: luemerumarco@yahoo.e [Universidad Centroccidental Lisandro Alvarado, Dpto. Quimica y Suelos, Decanato de Agronomia, Tarabana, Cabudare, Edo.Lara (Venezuela, Bolivarian Republic of); Bennun, Leonardo [Universidad de Concepcion, Concepcion (Chile); Greaves, Eduardo D. [Laboratorio de Fisica Nuclear, Dpto. De Fisica, Universidad Simon Bolivar, Sartenejas, Baruta (Venezuela, Bolivarian Republic of)

    2010-06-15

    The determination of arsenic in water samples requires techniques of high sensitivity. Total Reflection X-Ray Fluorescence (TXRF) allows the determination but a prior separation and pre-concentration procedure is necessary. Alumina is a suitable substrate for the selective separation of the analytes. A method for separation and pre-concentration in alumina, followed by direct analysis of the alumina is evaluated. Quantification was performed using the Al-K{alpha} and Co-K{alpha} lines as internal standard in samples prepared on an alumina matrix, and compared to a calibration with aqueous standards. Artificial water samples of As (III) and As (V) were analyzed after the treatment. Fifty milliliters of the sample at ppb concentration levels were mixed with 10 mg of alumina. The pH, time and temperature were controlled. The alumina was separated from the slurry by centrifugation, washed with de-ionized water and analyzed directly on the sample holder. A pre-concentration factor of 100 was found, with detection limit of 0.7 {mu}gL{sup -1}. The percentage of recovery was 98% for As (III) and 95% for As (V) demonstrating the suitability of the procedure.

  20. Determination of arsenic in water samples by Total Reflection X-Ray Fluorescence using pre-concentration with alumina

    International Nuclear Information System (INIS)

    Barros, Haydn; Marco Parra, Lue-Meru; Bennun, Leonardo; Greaves, Eduardo D.

    2010-01-01

    The determination of arsenic in water samples requires techniques of high sensitivity. Total Reflection X-Ray Fluorescence (TXRF) allows the determination but a prior separation and pre-concentration procedure is necessary. Alumina is a suitable substrate for the selective separation of the analytes. A method for separation and pre-concentration in alumina, followed by direct analysis of the alumina is evaluated. Quantification was performed using the Al-Kα and Co-Kα lines as internal standard in samples prepared on an alumina matrix, and compared to a calibration with aqueous standards. Artificial water samples of As (III) and As (V) were analyzed after the treatment. Fifty milliliters of the sample at ppb concentration levels were mixed with 10 mg of alumina. The pH, time and temperature were controlled. The alumina was separated from the slurry by centrifugation, washed with de-ionized water and analyzed directly on the sample holder. A pre-concentration factor of 100 was found, with detection limit of 0.7 μgL -1 . The percentage of recovery was 98% for As (III) and 95% for As (V) demonstrating the suitability of the procedure.

  1. Inorganic pigment study of the San Pedro Gonzalez Telmo Sibyls using total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Vazquez, Cristina; Custo, Graciela; Barrio, Nestor; Burucua, Jose; Boeykens, Susana; Marte, Fernando

    2010-01-01

    This article describes the study carried out on a series of oil paintings on canvas from the eighteenth century that were restored at Centro de Produccion e Investigacion en Restauracion y Conservacion Artistica y Bibliografica - Tarea (CEIRCAB-Tarea), Buenos Aires, Argentina: the San Pedro Gonzalez Telmo Sibyls. Experimental study was undertaken to identify inorganic pigments and the technique used in their confection; and, in this way, try to add information about their local origin. Therefore special emphasis was put to infer technologies used in the manufacturing of these paintings. Elemental analysis was performed by total reflection X-ray fluorescence spectrometry (TXRF) and complemented by optical and polarized light microscopy. Microsampling was carefully done over areas of the paintings which were damaged and where a small additional loss will not be noticed. This investigation has shown that a variety of pigments were used, namely earth pigments (red and yellow ochres), white lead, vermilion, etc., and they were used either pure or in mixtures. This characterization helped conservators in their decisions regarding a better understanding of the deterioration processes. In addition, this research about the material composition allowed the art historians and restorers the possibility to obtain information about where, when or by whom The San Pedro Gonzalez Telmo Sibyls may have been painted.

  2. Total reflection X-ray fluorescence applied to the chemical elements analysis of the mate tea infusion (Ilex-paraguariensis)

    International Nuclear Information System (INIS)

    Lopes, Fabio; Appoloni, Carlos R.; Cunha, Richard M. da Silva e; Nascimento Filho, Virgilio Franco do

    2002-01-01

    The purpose was to evaluate simultaneously the chemical element concentrations from K to Sr (19≤Z≤38) range in six samples of mate tea (Ilex paraguariensis) infusion, commercially available in Paraguay and South of Brazil. The chemical analysis of this beverage has a great nutritional importance for the native people of these areas, due to their large daily consumption. For the determination of these elements the dry-ashing and total reflection X-rays fluorescence (TXRF) were used. The methodology showed limits of detection among 81 ng.mL-1 for K to 10 ng.mL -1 for Zn. Six infusion samples were prepared in triplicate, and the concentration was 3,8 to 10,2 μg.mL -1 for K, Ca and Mn, 0,21 to 1,07 μg. mL -1 for Fe and Zn and 0.03 to 0,17 μg.mL -1 for Ni, Cu, Br, Rb and Sr. The Mn and Ni concentrations are above the maximum permissible values for drinking water established by World Health Organization and Brazilian legislation (these organisms do not regulate the maximum permissible values for chemical elements in mate tea infusion). (author)

  3. Element determination in natural biofilms of mine drainage water by total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Mages, Margarete; Tuempling, Wolf von Jr.; Veen, Andrea van der; Baborowski, Martina

    2006-01-01

    Human impacts like mining activities lead to higher element concentration in surface waters. For different pollution levels, the consequences for aquatic organisms are not yet investigated in detail. Therefore, the aim of this investigation is to determine the influence of mining affected surface waters on biofilms. Elements like heavy metals can be absorbed on cell walls and on polymeric substances or enter the cytoplasm of the cells. Thus, they are important for the optimization of industrial biotechnological processes and the environmental biotechnology. Beyond this, biofilms can also play an important role in wastewater treatment processes and serve as bioindicators in the aquatic environment. The presented total reflection X-ray fluorescence spectroscopic investigation was performed to compare the element accumulation behavior of biofilms grown on natural or on artificial materials of drainage water affected by former copper mining activities. A high salt and heavy metal pollution is characteristic for the drainage water. For an assessment of these results, samples from stream Schlenze upstream the confluence with the drainage water, a small tributary of the Saale River in central Germany, were analyzed, too

  4. Detection and quantitative determination of heavy metals in electronic cigarette refill liquids using Total Reflection X-ray Fluorescence Spectrometry.

    Science.gov (United States)

    Kamilari, Eleni; Farsalinos, Konstantinos; Poulas, Konstantinos; Kontoyannis, Christos G; Orkoula, Malvina G

    2018-06-01

    Electronic cigarettes are considered healthier alternatives to conventional cigarettes containing tobacco. They produce vapor through heating of the refill liquids (e-liquids) which consist of propylene glycol, vegetable glycerin, nicotine (in various concentrations), water and flavoring agents. Heavy metals may enter the refill liquid during the production, posing a risk for consumer's health due to their toxicity. The objective of the present study was the development of a methodology for the detection and quantitative analysis of cadmium (Cd), lead (Pb), nickel (Ni), copper (Cu), arsenic (As) and chromium (Cr), employing Total Reflection X-Ray Fluorescence Spectroscopy (TXRF) as an alternative technique to ICP-MS or ICP-OES commonly used for this type of analysis. TXRF was chosen due to its advantages, which include short analysis time, promptness, simultaneous multi-element analysis capability and minimum sample preparation, low purchase and operational cost. The proposed methodology was applied to a large number of electronic cigarette liquids commercially available, as well as their constituents, in order to evaluate their safety. TXRF may be a valuable tool for probing heavy metals in electronic cigarette refill liquids to serve for the protection of human health. Copyright © 2018 Elsevier Ltd. All rights reserved.

  5. Total reflection x-ray fluorescence spectroscopy as a tool for evaluation of iron concentration in ferrofluids and yeast samples

    International Nuclear Information System (INIS)

    Kulesh, N.A.; Novoselova, I.P.; Safronov, A.P.; Beketov, I.V.; Samatov, O.M.; Kurlyandskaya, G.V.; Morozova, M.; Denisova, T.P.

    2016-01-01

    In this study, total reflection x-ray fluorescent (TXRF) spectrometry was applied for the evaluation of iron concentration in ferrofluids and biological samples containing iron oxide magnetic nanoparticles obtained by the laser target evaporation technique. Suspensions of maghemite nanoparticles of different concentrations were used to estimate the limitation of the method for the evaluation of nanoparticle concentration in the range of 1–5000 ppm in absence of organic matrix. Samples of single-cell yeasts grown in the nutrient media containing maghemite nanoparticles were used to study the nanoparticle absorption mechanism. The obtained results were analyzed in terms of applicability of TXRF for quantitative analysis in a wide range of iron oxide nanoparticle concentrations for biological samples and ferrofluids with a simple established protocol of specimen preparation. - Highlights: • Ferrofluids and yeasts samples were analysed by TXRF spectroscopy. • Simple protocol for iron quantification by means of TXRF was proposed. • Results were combined with magnetic, structural, and morphological characterization. • Preliminary conclusion on nanoparticles uptake mechanism was made.

  6. Use of total-reflection x-ray fluorescence in search of a biomonitor for environmental pollution in Vietnam

    International Nuclear Information System (INIS)

    Boman, J.; Wagner, A.; Brauer, H.; Viet Binh, D.

    2000-01-01

    The concentration of trace elements in tissues of several animals collected in the Ha Nam province, about 25 km south of Hanoi, Vietnam, has been investigated using total-reflection x-ray fluorescence (TXRF). With this study we wanted to address whether any of the animals were possible candidates for being bio-monitors for the pollution situation in a selected area of Vietnam. We also aim to compare the measured trace element concentrations to those representative to other provinces in Vietnam as well as to other parts of the world. An extensive bio-diversity of animals exists in Vietnam, where many of them play an important economic role in the agricultural breeding and production. The accumulation process of trace elements is still not known for a large number of animals. The parts of the collected animals chosen for analysis were muscle tissue and liver. The specimens were dried under vacuum and kept frozen. Before the TXRF analysis, the solid and dried samples were digested in nitric acid. The analysis was made at the Department of Physics at Chalmers University of Technology and Goeteborg University, Sweden, where a TXRF spectrometer has been developed by the Environmental Physics group. The results show that there could be a large variation in the concentration of trace elements, not only between the different animals but also between tissue parts of the same animal. Obviously, when selecting an organism to be used as a bio-monitor, other factors than the mere concentration of trace elements must be considered. (author)

  7. Total reflection X-ray fluorescence analysis of oral fluids of women affected by osteoporosis and osteopenia

    Science.gov (United States)

    Sánchez, Héctor Jorge; Valentinuzzi, María Cecilia; Grenón, Miram; Abraham, José

    2008-12-01

    Osteoporosis is a disease characterized by low bone mass and microarchitectural deterioration of bone tissue, leading to bone fragility and an increased susceptibility to fractures; the early stage of decreased bone density is called osteopenia. More than 200 million people are affected and about 50% of post-menopausic women are expected to develop the disease. Osteoporosis, osteopenia and periodontal disease have in common several risk factors, being hyperthyroidism and smoking habits the most important ones. There is scarce information in the literature about the association between periodontal disease and osteoporosis and/or osteopenia. Some works suggest that osteoporotic women are susceptible to a higher loss of periodontal insertion, alveolar bones, and teeth. Thirty adult post-menopausic women were studied; some of them were healthy (control group) and the rest of them were undergoing some stage of osteoporosis or osteopenia. All the subjects were healthy, non-smokers, not having dental implants, and with communitarian periodontal index higher than 1(CPI > 1). Samples of saliva and gingival crevice fluid were extracted with calibrated micro-capillaries and deposited on Si reflectors. Known amounts of Ga were added to the samples in order to act as internal standard for quantification by the total reflection x-ray fluorescence technique. Experimental concentrations of several elements (P, S, Cl, K, Ca, Cr, Fe, NI, Cu, and Zn) were determined. The concentration of some elements in saliva showed different behavior as compared to gingival crevice fluid. Some critical elements of bone composition, such as Ca and Zn, present very distinguishable behavior. Improvements in the statistics are required for a better assessment of a routine method and to establish some correlation with periodontal disease. TXRF seems to be a promising method to evaluate the evolution of osteoporosis.

  8. Vapor phase treatment–total reflection X-ray fluorescence for trace elemental analysis of silicon wafer surface

    International Nuclear Information System (INIS)

    Takahara, Hikari; Mori, Yoshihiro; Shibata, Harumi; Shimazaki, Ayako; Shabani, Mohammad B.; Yamagami, Motoyuki; Yabumoto, Norikuni; Nishihagi, Kazuo; Gohshi, Yohichi

    2013-01-01

    Vapor phase treatment (VPT) was under investigation by the International Organization for Standardization/Technical Committee 201/Working Group 2 (ISO/TC201/WG2) to improve the detection limit of total reflection X-ray fluorescence spectroscopy (TXRF) for trace metal analysis of silicon wafers. Round robin test results have confirmed that TXRF intensity increased by VPT for intentional contamination with 5 × 10 9 and 5 × 10 10 atoms/cm 2 Fe and Ni. The magnification of intensity enhancement varied greatly (1.2–4.7 in VPT factor) among the participating laboratories, though reproducible results could be obtained for average of mapping measurement. SEM observation results showed that various features, sizes, and surface densities of particles formed on the wafer after VPT. The particle morphology seems to have some impact on the VPT efficiency. High resolution SEM observation revealed that a certain number of dots with SiO 2 , silicate and/or carbon gathered to form a particle and heavy metals, Ni and Fe in this study were segregated on it. The amount and shape of the residue should be important to control VPT factor. - Highlights: • This paper presents a summary of study results of VPT–TXRF using ISO/TC201/WG2. • Our goal is to analyze the trace metallic contamination on silicon wafer with concentrations below 1 × 10 10 atoms/cm 2 . • The efficiency and mechanism of VPT are discussed under several round robin tests and systematic studies

  9. Determination of As concentration in earthworm coelomic fluid extracts by total-reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Allegretta, Ignazio; Porfido, Carlo; Panzarino, Onofrio; Fontanella, Maria Chiara; Beone, Gian Maria; Spagnuolo, Matteo; Terzano, Roberto

    2017-04-01

    Earthworms are often used as sentinel organisms to study As bioavailability in polluted soils. Arsenic in earthworms is mainly sequestrated in the coelomic fluids whose As content can therefore be used to asses As bioavalability. In this work, a method for determining As concentration in coelomic fluid extracts using total-reflection X-ray fluorescence spectrometry (TXRF) is presented. For this purpose coelomic fluid extracts from earthworms living in three polluted soils and one non-polluted (control) soil have been collected and analysed. A very simple sample preparation was implemented, consisting of a dilution of the extracts with polyvinyl alcohol (PVA) using a 1:8 ratio and dropwise deposition of the sample on the reflector. A detection limit of 0.2 μg/l and quantification limit of 0.6 μg/l was obtained in the diluted samples, corresponding to 2 μg/l and 6 μg/l in the coelomic fluid extracts, respectively. This allowed to quantify As concentration in coelomic fluids extracted from earthworms living in soils polluted with As at concentrations higher than 20 mg/kg (considered as a pollution threshold for agricultural soils). The TXRF method has been validated by comparison with As concentrations in standards and by analysing the same samples by ICP-MS, after acid digestion of the sample. The low limit of detection, the proven reliability of the method and the little sample preparation make TXRF a suitable, cost-efficient and "green" technique for the analysis of As in earthworm coelomic fluid extracts for bioavailability studies.

  10. Total reflection X-ray fluorescence analysis of oral fluids of women affected by osteoporosis and osteopenia

    International Nuclear Information System (INIS)

    Sanchez, Hector Jorge; Valentinuzzi, Maria Cecilia; Grenon, Miram; Abraham, Jose

    2008-01-01

    Osteoporosis is a disease characterized by low bone mass and microarchitectural deterioration of bone tissue, leading to bone fragility and an increased susceptibility to fractures; the early stage of decreased bone density is called osteopenia. More than 200 million people are affected and about 50% of post-menopausic women are expected to develop the disease. Osteoporosis, osteopenia and periodontal disease have in common several risk factors, being hyperthyroidism and smoking habits the most important ones. There is scarce information in the literature about the association between periodontal disease and osteoporosis and/or osteopenia. Some works suggest that osteoporotic women are susceptible to a higher loss of periodontal insertion, alveolar bones, and teeth. Thirty adult post-menopausic women were studied; some of them were healthy (control group) and the rest of them were undergoing some stage of osteoporosis or osteopenia. All the subjects were healthy, non-smokers, not having dental implants, and with communitarian periodontal index higher than 1(CPI > 1). Samples of saliva and gingival crevice fluid were extracted with calibrated micro-capillaries and deposited on Si reflectors. Known amounts of Ga were added to the samples in order to act as internal standard for quantification by the total reflection x-ray fluorescence technique. Experimental concentrations of several elements (P, S, Cl, K, Ca, Cr, Fe, NI, Cu, and Zn) were determined. The concentration of some elements in saliva showed different behavior as compared to gingival crevice fluid. Some critical elements of bone composition, such as Ca and Zn, present very distinguishable behavior. Improvements in the statistics are required for a better assessment of a routine method and to establish some correlation with periodontal disease. TXRF seems to be a promising method to evaluate the evolution of osteoporosis

  11. Determination of trace elements in freshwater rotifers and ciliates by total reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Woelfl, S.; Óvári, M.; Nimptsch, J.; Neu, T. R.; Mages, M.

    2016-02-01

    Element determination in plankton is important for the assessment of metal contamination of aquatic environments. Until recently, it has been difficult to determine elemental content in rotifers or ciliates derived from natural plankton samples because of the difficulty in handling and separation of these fragile organisms. The aim of this study was to evaluate methods for separation of rotifers and large ciliates from natural plankton samples (μg range dry weight) and subsequent analysis of their elemental content using total-reflection X-ray fluorescence spectrometry (TXRF). Plankton samples were collected from different aquatic environments (three lakes, one river) in Chile, Argentina and Hungary. From one to eighty specimens of five rotifer species (Brachionus calyciflorus, Brachionus falcatus, Asplanchna sieboldii, Asplanchna sp., Philodina sp.) and four to twelve specimens of one large ciliate (Stentor amethystinus) were prepared according to the dry method originally developed for microcrustaceans, and analysed by TRXF following in situ microdigestion. Our results demonstrated that it possible to process these small and fragile organisms (individual dry mass: 0.17-9.39 μg ind- 1) via careful washing and preparation procedures. We found species-dependent differences of the element mass fractions for some of the elements studied (Cr, Mn, Fe, Ni, Cu, Zn, As, Pb), especially for Cu, Fe and Mn. One large rotifer species (A. sieboldii) also showed a negative correlation between individual dry weight and the element content for Pb, Ni and Cr. We conclude that our application of the in situ microdigestion-TRXF method is suitable even for rotifers and ciliates, greatly expanding the possibilities for use of plankton in biomonitoring of metal contamination in aquatic environments.

  12. Total reflection X-ray fluorescence analysis of oral fluids of women affected by osteoporosis and osteopenia

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez, Hector Jorge [Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina)], E-mail: jsan@famaf.unc.edu.ar; Valentinuzzi, Maria Cecilia [Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina); Grenon, Miram [Facultad de Odontologia, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina); Abraham, Jose [Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina)

    2008-12-15

    Osteoporosis is a disease characterized by low bone mass and microarchitectural deterioration of bone tissue, leading to bone fragility and an increased susceptibility to fractures; the early stage of decreased bone density is called osteopenia. More than 200 million people are affected and about 50% of post-menopausic women are expected to develop the disease. Osteoporosis, osteopenia and periodontal disease have in common several risk factors, being hyperthyroidism and smoking habits the most important ones. There is scarce information in the literature about the association between periodontal disease and osteoporosis and/or osteopenia. Some works suggest that osteoporotic women are susceptible to a higher loss of periodontal insertion, alveolar bones, and teeth. Thirty adult post-menopausic women were studied; some of them were healthy (control group) and the rest of them were undergoing some stage of osteoporosis or osteopenia. All the subjects were healthy, non-smokers, not having dental implants, and with communitarian periodontal index higher than 1(CPI > 1). Samples of saliva and gingival crevice fluid were extracted with calibrated micro-capillaries and deposited on Si reflectors. Known amounts of Ga were added to the samples in order to act as internal standard for quantification by the total reflection x-ray fluorescence technique. Experimental concentrations of several elements (P, S, Cl, K, Ca, Cr, Fe, NI, Cu, and Zn) were determined. The concentration of some elements in saliva showed different behavior as compared to gingival crevice fluid. Some critical elements of bone composition, such as Ca and Zn, present very distinguishable behavior. Improvements in the statistics are required for a better assessment of a routine method and to establish some correlation with periodontal disease. TXRF seems to be a promising method to evaluate the evolution of osteoporosis.

  13. Application of CO2 Snow Jet Cleaning in Conjunction with Laboratory Based Total Reflection X-Ray Fluorescence

    Science.gov (United States)

    Schmeling, M.; Burnett, D. S.; Allton, J. H.; Rodriquez, M.; Tripa, C. E.; Veryovkin, I. V.

    2013-01-01

    The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.

  14. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    International Nuclear Information System (INIS)

    Marguí, Eva; Queralt, Ignasi; Hidalgo, Manuela

    2013-01-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2–4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods. - Highlights: • A TXRF method for PGM catalyst residue determination in API samples is presented. • Analysis can be performed using 10 μL of the internal standardized dissolved API. • The method is rapid, simple and suitable according to the USP requirements

  15. X-ray reflectivity and surface roughness

    International Nuclear Information System (INIS)

    Ocko, B.M.

    1988-01-01

    Since the advent of high brightness synchrotron radiation sources there has been a phenomenal growth in the use of x-rays as a probe of surface structure. The technique of x-ray reflectivity is particularly relevant to electrochemists since it is capable of probing the structure normal to an electrode surface in situ. In this paper the theoretical framework for x-ray reflectivity is reviewed and the results from previous non-electrochemistry measurements are summarized. These measurements are from the liquid/air interface (CCl 4 ), the metal crystal vacuum interface (Au(100)), and from the liquid/solid interface(liquid crystal/silicon). 34 refs., 5 figs

  16. Total reflection x-ray fluorescence (TXRF) - a tool to obtain information about different air masses and air pollution

    International Nuclear Information System (INIS)

    Schmeling, M.

    2000-01-01

    Aerosols are solid particles dissolved in the atmosphere and have strong influence in the earth climate. Their solid surfaces are the only atmospheric medium for condensation of water leading to cloud formation and ultimately to precipitation. Besides their role in cloud formation, the elemental composition of aerosols reveals useful information about air masses and their transport patterns as well as air pollution. The elemental composition can be considered like a fingerprint of an air mass telling the story about its origin and fate. The presence of Al, Ti and Fe for instance indicates a source located in a highly exposed soil or often desert region, whereas Ni, V and Pb can be traced back to anthropogenic activities like fuel combustion or industrial processes. Other important source regions are the oceans, which emit the main aerosol constituents Na, Cl, and S. The concentrations of these elements in the atmosphere are extremely low and long sampling times are necessary to gain reliable results with most of the common analysis techniques. In contrast to this total reflection x-ray fluorescence (TXRF), as a technique capable to cope with tiny sample amounts, offers the unique possibility to reduce collection times to a minimum of minutes to hours. Such short sampling times in turn render it possible to monitor different air masses either passing through a ground based station or -in the ideal case- flown into by a small research aircraft. Different aerosol samples were taken by aircraft during the second aerosol characterization experiment (ACE-2) with sampling times ranging from 15 minutes up to one hour. These filter samples were analyzed by TXRF for trace elements subsequently. Together with background information about back trajectories and size distribution covering the time of sampling the presence of different air masses could be detected. In another project, short-term samples in the Chicago/Lake Michigan area are collected to study the air mass

  17. Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Amberger, Martin A.; Hoeltig, Michael; Broekaert, Jose A.C.

    2010-01-01

    The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1 . As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g -1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2 O 3 , powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a

  18. Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Amberger, Martin A.; Hoeltig, Michael [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C., E-mail: jose.broekaert@chemie.uni-hamburg.d [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

    2010-02-15

    The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL{sup -1}. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL{sup -1} of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 mug g{sup -1} for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al{sub 2}O{sub 3}, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective

  19. Determination of total As in onion plants growing in contaminated substrates by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Lue-Meru Marco Parra

    2011-01-01

    The onion (Allium cepa L.) is one of the most important cultivars in the world and its production level occupies the second place in Venezuela. It becomes important to develop analytical procedures for arsenic determination and to study the effect of this element on the cultures, as well the absorption, transport and translocation processes. A TXRF method for As determination in onions was developed. Two treatments were applied to the onion plants, As contaminated and control. The contaminant was added to the plants to an amount of 100 μg, in a single time 3 weeks after the transplant of plantlets. The green leaves bulbs, and roots together with the stems were separated 45 days after transplant and analyzed by TXRF and HG-AAS for total Arsenic determination. A good agreement was found between these two techniques, demonstrating the accuracy of the TXRF procedure. It was found that the highest concentration corresponded to the root and stems (37 ± 31 μg g -1 ), followed by the bulbs (11 ± 7 μg g -1 ), being the smallest level found in the green leaves (4 ± 3 μg g -1 ). At low As contamination levels of 0.25 μg g -1 , a risk for translocation of the toxic element to the edible parts of the onion plants exists. At this level the normal development of the plant is not affected, being the only exception the root length, which is significantly higher in the contaminated treatment. (author)

  20. Matrix effect on the detection limit and accuracy in total reflection X-ray fluorescence analysis of trace elements in environmental and biological samples

    International Nuclear Information System (INIS)

    Karjou, J.

    2007-01-01

    The effect of matrix contents on the detection limit of total reflection X-ray fluorescence analysis was experimentally investigated using a set of multielement standard solutions (500 ng/mL of each element) in variable concentrations of NH 4 NO 3 . It was found that high matrix concentration, i.e. 0.1-10% NH 4 NO 3 , had a strong effect on the detection limits for all investigated elements, whereas no effect was observed at lower matrix concentration, i.e. 0-0.1% NH 4 NO 3 . The effect of soil and blood sample masses on the detection limit was also studied. The results showed decreasing the detection limit (in concentration unit, μg/g) with increasing the sample mass. However, the detection limit increased (in mass unit, ng) with increasing sample mass. The optimal blood sample mass of ca. 200 μg was sufficient to improve the detection limit of Se determination by total reflection X-ray fluorescence. The capability of total reflection X-ray fluorescence to analyze different kinds of samples was discussed with respect to the accuracy and detection limits based on certified and reference materials. Direct analysis of unknown water samples from several sources was also presented in this work

  1. Analysis of total and dissolved heavy metals in surface water of a Mexican polluted river by total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zarazua, G. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico)]. E-mail: gzo@nuclear.inin.mx; Avila-Perez, P. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Tejeda, S. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Barcelo-Quintal, I. [Universidad Autonoma Metropolitana, Unidad Azcapotzalco, Mexico, D.F. (Mexico); Martinez, T. [Universidad Nacional Autonoma de Mexico, Facultad de Quimica, Mexico, D.F. (Mexico)

    2006-11-15

    The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 {mu}g/L) > Mn (300 {mu}g/L) > Cu (66 {mu}g/L) > Cr (21 {mu}g/L) > Pb (15 {mu}g/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits.

  2. Analysis of total and dissolved heavy metals in surface water of a Mexican polluted river by total reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Zarazua, G.; Ávila-Pérez, P.; Tejeda, S.; Barcelo-Quintal, I.; Martínez, T.

    2006-11-01

    The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 μg/L) > Mn (300 μg/L) > Cu (66 μg/L) > Cr (21 μg/L) > Pb (15 μg/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits.

  3. Analysis of total and dissolved heavy metals in surface water of a Mexican polluted river by total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Zarazua, G.; Avila-Perez, P.; Tejeda, S.; Barcelo-Quintal, I.; Martinez, T.

    2006-01-01

    The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 μg/L) > Mn (300 μg/L) > Cu (66 μg/L) > Cr (21 μg/L) > Pb (15 μg/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits

  4. Monitoring environmental pollution of trace elements in tree-rings by synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    International Nuclear Information System (INIS)

    Moreira, Silvana; Vives, Ana Elisa S. de; Brienza, Sandra Maria B.; Medeiros, Jean Gabriel S.; Tomazello Filho, Mario; Zucchi, Orgheda L.A.D.; Nascimento Filho, Virgilio F.

    2005-01-01

    This paper aims to study the environmental pollution in the tree development, as a manner to evaluate its use as bioindicator in urban and country sides. The sample collecting was carry out in Piracicaba city, Sao Paulo State, that presents high level of environmental contamination of the water, soil and air, due industrial activities, vehicles combustion, sugar-cane leaves burning in the harvesting, etc. It was selected the Caesalpinia peltophoroides ('Sibipiruna') specie because its very used in urban arborization. It was employed the analytical technique named total reflection X-ray fluorescence (TXRF) to identify and quantify the elements and metals of nutritional and toxicological importance in the wood samples. The analysis was done in the Brazilian Synchrotron Light Laboratory, using a white beam for excitation and a Si(Li) detector for characteristic X-ray detection. It was quantified the P, K, Ca, Ti, Fe, Sr, Ba e Pb elements. (author)

  5. Monitoring environmental pollution of trace elements in tree-rings by synchrotron radiation total reflection X-ray fluorescence analysis (SR-TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Brienza, Sandra Maria B. [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil) Faculdade de Ciencias Matematicas, da Natureza e de Tecnologia da Informacao]. E-mail: sbrienza@unimep.br; Medeiros, Jean Gabriel S.; Tomazello Filho, Mario [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz]. E-mail: jeangm@esalq.usp.br; mtomazel@esalq.usp.br; Zucchi, Orgheda L.A.D. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br

    2005-07-01

    This paper aims to study the environmental pollution in the tree development, as a manner to evaluate its use as bioindicator in urban and country sides. The sample collecting was carry out in Piracicaba city, Sao Paulo State, that presents high level of environmental contamination of the water, soil and air, due industrial activities, vehicles combustion, sugar-cane leaves burning in the harvesting, etc. It was selected the Caesalpinia peltophoroides ('Sibipiruna') specie because its very used in urban arborization. It was employed the analytical technique named total reflection X-ray fluorescence (TXRF) to identify and quantify the elements and metals of nutritional and toxicological importance in the wood samples. The analysis was done in the Brazilian Synchrotron Light Laboratory, using a white beam for excitation and a Si(Li) detector for characteristic X-ray detection. It was quantified the P, K, Ca, Ti, Fe, Sr, Ba e Pb elements. (author)

  6. Quantitative determination of iron, copper, lead, chromium and nickel in electronic waste samples using total reflection x-ray fluorescence spectroscopy

    International Nuclear Information System (INIS)

    Elaseer, A. S.; Musbah, A. S; Ammar, M. M. G.; Salah, M. A.; Aisha, E. A.

    2015-01-01

    Total reflection x-ray fluorescence spectroscopy in conjunction with microwave assisted extraction technique was used for the analysis of twenty electronic waste samples. The analysis was limited to the printed circuit boards of electronic devices. Iron, copper, lead, chromium and nickel were quantitatively determined in the samples. The samples were carefully milled to fine powder and 50mg was digested by acid using microwave digestion procedure. The digested samples solution was spread together with gallium as internal standard on the reflection disk and analyzed. The results showed that the cassette recorder boards contain the highest concentration of iron, lead and nickel. The average concentrations of these metals were 78, 73 and 71g/Kg respectively. Computer boards contained the highest copper average concentration 39g/Kg. the highest chromium average concentration 3.6 g/Kg was in mobile phone boards. Measurements were made using PicoTAX portable x-ray device. the instrument was used for quantitative multi-element analysis. An air cooled x-ray tube (40KV, 1 mA) with Mo target and Be window was used as x-ray source. The optics of the device was a multilayer Ni/C, 17.5 keV, 80% reflectivity provides analysis of elements from Si to Zr (K series) and Rh to U (L series). A Si PIN-diode detector (7mm"2, 195eV) was used for the elements detection. In this study heavy metals average concentration in electronic circuit boards in the in the order of iron (35.25g/kg), copper (21.14g/Kg), lead (16.59g/Kg), nickel (16.01g/Kg) and chromium (1.07g/Kg).(author)

  7. Quantitative determination on heavy metals in different stages of wine production by Total Reflection X-ray Fluorescence and Energy Dispersive X-ray Fluorescence: Comparison on two vineyards

    Energy Technology Data Exchange (ETDEWEB)

    Pessanha, Sofia [Centro Fisica Atomica, Departamento de Fisica, Faculdade de Ciencias, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003 Lisboa (Portugal); Carvalho, Maria Luisa, E-mail: luisa@cii.fc.ul.p [Centro Fisica Atomica, Departamento de Fisica, Faculdade de Ciencias, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003 Lisboa (Portugal); Becker, Maria; Bohlen, Alex von [Institute for analytical Sciences, Bunsen-Kirchhoff-Str. 11, 44139 Dortmund (Germany)

    2010-06-15

    The purpose of this study is to determine the elemental content, namely heavy metals, of samples of vine-leaves, grapes must and wine. In order to assess the influence of the vineyard age on the elemental content throughout the several stages of wine production, elemental determinations of trace elements were made on products obtained from two vineyards aged 6 and 14 years from Douro region. The elemental content of vine-leaves and grapes was determined by Energy Dispersive X-Ray Fluorescence (EDXRF), while analysis of the must and wine was performed by Total Reflection X-ray Fluorescence (TXRF). Almost all elements present in wine and must samples did not exceed the recommended values found in literature for wine. Bromine was present in the 6 years old wine in a concentration 1 order of magnitude greater than what is usually detected. The Cu content in vine-leaves from the older vineyard was found to be extremely high probably due to excessive use of Cu-based fungicides to control vine downy mildew. Higher Cu content was also detected in grapes although not so pronounced. Concerning the wine a slightly higher level was detected on the older vineyard, even so not exceeding the recommended value.

  8. Quantitative determination on heavy metals in different stages of wine production by Total Reflection X-ray Fluorescence and Energy Dispersive X-ray Fluorescence: Comparison on two vineyards

    International Nuclear Information System (INIS)

    Pessanha, Sofia; Carvalho, Maria Luisa; Becker, Maria; Bohlen, Alex von

    2010-01-01

    The purpose of this study is to determine the elemental content, namely heavy metals, of samples of vine-leaves, grapes must and wine. In order to assess the influence of the vineyard age on the elemental content throughout the several stages of wine production, elemental determinations of trace elements were made on products obtained from two vineyards aged 6 and 14 years from Douro region. The elemental content of vine-leaves and grapes was determined by Energy Dispersive X-Ray Fluorescence (EDXRF), while analysis of the must and wine was performed by Total Reflection X-ray Fluorescence (TXRF). Almost all elements present in wine and must samples did not exceed the recommended values found in literature for wine. Bromine was present in the 6 years old wine in a concentration 1 order of magnitude greater than what is usually detected. The Cu content in vine-leaves from the older vineyard was found to be extremely high probably due to excessive use of Cu-based fungicides to control vine downy mildew. Higher Cu content was also detected in grapes although not so pronounced. Concerning the wine a slightly higher level was detected on the older vineyard, even so not exceeding the recommended value.

  9. Determination of ultra trace contaminants on silicon wafer surfaces using total-reflection X-ray fluorescence TXRF 'state-of-the-art'

    Science.gov (United States)

    Pahlke, S.; Fabry, L.; Kotz, L.; Mantler, C.; Ehmann, T.

    2001-11-01

    In a well balanced system of highly motivated, well trained personnel and automated equipment, pure reagents and bulk media, cleanrooms and integrated data management, total-reflection X-ray fluorescence (TXRF) can and must contribute to quality assurance and process stability, support and canalize creative engineering by continuous learning about materials and processes. TXRF has the advantage of controlled one-point calibration, a linear dynamic range of three orders of magnitude, high grade of automation in operation and data management, high up-time, and a simple control of data plausibility.

  10. Multielement determination in river-water of Sepetiba Bay tributaries (Brazil) by total reflection X-ray fluorescence using synchrotron radiation

    International Nuclear Information System (INIS)

    Costa, A.C.M.; Castro, C.R.F.; Lopes, R.T.; Anjos, M.J.; Rio de Janeiro State Univ.

    2006-01-01

    Trace elements were determined in the surface waters of tributaries of the Sepetiba Bay, Brazil (Piraque, Ita, Sao Francisco, Guarda, Guandu Mirim, Vala do Sangue and Engenho Novo rivers) by total reflection X-ray fluorescence using synchrotron radiation (SRTXRF). Eighteen trace elements could be determined in the dissolved and the suspended particulate phases: Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Br, Rb, Sr and Pb. The elemental concentration values were compared to the values recommended by the Brazilian legislation. (author)

  11. Hygrothermal degradation of (3-glycidoxypropyl)trimethoxysilane films studied by neutron and X-ray reflectivity and attenuated total reflection infrared spectroscopy

    International Nuclear Information System (INIS)

    Tallant, David Robert; Garcia, Manuel Joseph; Majewski, Jaroslaw; Kent, Michael Stuart; Yim, Hyun

    2005-01-01

    Thin films of organosilanes have great technological importance in the areas of adhesion promotion, durability, and corrosion resistance. However, it is well-known that water can degrade organosilane films, particularly at elevated temperatures. In this work, X-ray and neutron reflectivity (XR and NR) were combined with attenuated total reflection infrared (ATR-IR) spectroscopy to study the chemical and structural changes within thin films of (3-glycidoxypropyl)trimethoxysilane (GPS) after exposure for various periods of time to air saturated with either D 2 O or H 2 O at 80 C. For NR and XR, ultrathin (∼100 (angstrom)) films were prepared by spin-coating. Both D 2 O and H 2 O provide neutron scattering contrast with GPS. Variations in the neutron scattering length density (SLD) profiles (a function of mass density and atomic composition) with conditioning time were measured after drying the samples out and also swelled with H 2 O or D 2 O vapor at room temperature. For samples that were dried out prior to measurement, little or no change was observed for H 2 O conditioning up to 3.5 days, but large changes were observed after 30 days of conditioning. The range of conditioning time for this structural change was narrowed to between 4 and 10 days with XR. The SLD profiles indicated that the top portion of the GPS film was transformed into a thick low-density layer after conditioning, but the bottom portion showed little structural change. A previous NR study of as-prepared GPS films involving swelling with deuterated nitrobenzene showed that the central portion of the film has much lower cross-link density than the region nearest the substrate. The present data show that the central portion also swells to a much greater extent with water and hydrolyzes more rapidly. The chemical degradation mechanism was identified by IR as hydrolysis of siloxane bonds. For ATR-IR, GPS films were prepared by dip-coating, which resulted in a greater and more variable thickness than

  12. Total external reflection X-ray fluorescence analysis of protein-metal ion interactions in biological systems

    Science.gov (United States)

    Novikova, N. N.; Kovalchuk, M. V.; Yur'eva, E. A.; Konovalov, O. V.; Rogachev, A. V.; Stepina, N. D.; Sukhorukov, V. S.; Tsaregorodtsev, A. D.; Chukhrai, E. S.; Yakunin, S. N.

    2012-09-01

    This paper presents the results of an investigation into hemoglobin-based protein films that were formed on a liquid surface. X-ray standing wave measurements were performed at the ID 10 beamline of the European Synchrotron Radiation Facility (ESRF) and at the Langmuir station of the Kurchatov Synchrotron Radiation Source. It was found that the ability of the protein to bind metal ions is substantially increased due to the conformational rearrangements of protein macromolecules caused by various damaging effects. The elemental composition of protein preparations, which were isolated from children and adults with chronic metabolic diseases accompanied by endogenous intoxication, was analyzed. The results of the investigations offer evidence that an increase in the ligand-binding properties of the protein molecules, which was observed in model experiments using protein films, is a common trait and corresponds to in vivo processes accompanying metabolic disturbances in the body.

  13. Determination of lead in clay enameled by X-ray fluorescence technique in Total reflection and by Scanning Electron Microscopy; Determinacion de plomo en esmaltado de barro por Fluorescencia de rayos X en reflexion total y Microscopia Electronica de Barrido

    Energy Technology Data Exchange (ETDEWEB)

    Zarazua O, G.; Carapia M, L. [Instituto Nacional de Investigaciones Nucleares, C.P. 52045 Estado de Mexico (Mexico)

    2000-07-01

    This work has the objective of determining lead free in the glazed commercial stewing pans using the X-ray fluorescence technique in Total reflection (FRX) and the observation and semiquantitative determination of lead by Analytical Scanning Electron Microscopy (ASEM). (Author)

  14. Evaluation of heavy metals in atmospheric emissions from automotive industry by total reflection X-ray fluorescence with synchrotron radiation

    International Nuclear Information System (INIS)

    Moreira, Silvana; Weber Neto, Jose; Vives, Ana Elisa Sirito de

    2009-01-01

    This study had as goal to determine heavy metals and other elements (Ba, Br, Ca, Pb, Cl, Cr, Sr, Fe, Mn, Ni, K, Si, Ti and Zn) in atmospheric pollutants generated by an automotive industry located in the city of Engenheiro Coelho, state of Sao Paulo, Brazil. The sampling and sample preparation procedures were based on methods established by the Company of Sanitation and Technology (CETESB L9.234) and also by the Environmental Protection Agency (EPA - Method 29). The analysis was performed at XRF Beamline (D09B-XRF) in the Synchrotron Light Source Laboratory (Campinas/SP). A white beam of synchrotron radiation was used for sample and standard excitation which were irradiated by 100 seconds. For X-ray lines detection, a Ge (HP) detector with 150 eV of resolution at 5.9 keV was employed. For zinc, iron, barium, calcium and potassium, the values obtained were in the range of 30 mg/Nm 3 and, for other elements, the concentrations were approximately 1 mg/Nm 3 . The sum of As, Be, Co, Cr, Cu, Mn, Ni, Pb, Sb, Se, Sn, Te and Zn concentration was compared with the limits established by CONAMA 264/1999 and SEMA 041/2002 resolutions (7.0 mg/Nm 3 ) and it was observed that, for all samples, sums are higher than the permissive value mainly due to the high concentration of zinc. Detection limits for SR-TXRF technique were 0.10 μg/Nm 3 for Pb and 0.02 μg/Nm 3 for Zn. (author)

  15. Evaluation of heavy metals in atmospheric emissions from automotive industry by total reflection X-ray fluorescence with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Weber Neto, Jose, E-mail: silvana@fec.unicamp.b [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Saneamento e Ambiente; Vives, Ana Elisa Sirito de, E-mail: aesvives@unimep.b [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo

    2009-07-01

    This study had as goal to determine heavy metals and other elements (Ba, Br, Ca, Pb, Cl, Cr, Sr, Fe, Mn, Ni, K, Si, Ti and Zn) in atmospheric pollutants generated by an automotive industry located in the city of Engenheiro Coelho, state of Sao Paulo, Brazil. The sampling and sample preparation procedures were based on methods established by the Company of Sanitation and Technology (CETESB L9.234) and also by the Environmental Protection Agency (EPA - Method 29). The analysis was performed at XRF Beamline (D09B-XRF) in the Synchrotron Light Source Laboratory (Campinas/SP). A white beam of synchrotron radiation was used for sample and standard excitation which were irradiated by 100 seconds. For X-ray lines detection, a Ge (HP) detector with 150 eV of resolution at 5.9 keV was employed. For zinc, iron, barium, calcium and potassium, the values obtained were in the range of 30 mg/Nm{sup 3} and, for other elements, the concentrations were approximately 1 mg/Nm{sup 3}. The sum of As, Be, Co, Cr, Cu, Mn, Ni, Pb, Sb, Se, Sn, Te and Zn concentration was compared with the limits established by CONAMA 264/1999 and SEMA 041/2002 resolutions (7.0 mg/Nm{sup 3}) and it was observed that, for all samples, sums are higher than the permissive value mainly due to the high concentration of zinc. Detection limits for SR-TXRF technique were 0.10 mug/Nm{sup 3} for Pb and 0.02 mug/Nm{sup 3} for Zn. (author)

  16. Monitoring of the environmental pollution by trace element analysis in tree-rings using synchrotron radiation total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Sirito de Vives, Ana Elisa [School of Civil Engineering, Architecture and Urban Design Methodist University of Piracicaba, Rodovia Santa Barbara D' Oeste/Iracemapolis, km 01, 13450-000 Santa Barbara D' Oeste, SP (Brazil)]. E-mail: aesvives@unimep.br; Moreira, Silvana [State University of Campinas - UNICAMP/FEC (Brazil); Brienza, Sandra Maria Boscolo [School of Civil Engineering, Architecture and Urban Design Methodist University of Piracicaba, Rodovia Santa Barbara D' Oeste/Iracemapolis, km 01, 13450-000 Santa Barbara D' Oeste, SP (Brazil); Silva Medeiros, Jean Gabriel [University of Sao Paulo - USP/ ESALQ (Brazil); Tomazello Filho, Mario Tomazello [University of Sao Paulo - USP/ ESALQ (Brazil); Araujo Domingues Zucchi, Orgheda Luiza [University of Sao Paulo - USP/FCFRP (Brazil); Nascimento Filho, Virgilio Franco do [University of Sao Paulo - USP/CENA (Brazil)

    2006-11-15

    This paper aims to study the environmental pollution in the tree development, in order to evaluate its use as bioindicator in urban and country sides. The sample collection was carried out in Piracicaba city, Sao Paulo State, which presents high level of environmental contamination in water, soil and air, due to industrial activities, vehicles combustion, sugar-cane leaves burning in the harvesting, etc. The species Caesalpinia peltophoroides ('Sibipiruna') was selected because it is widely used in urban forestation. Synchrotron Radiation Total Reflection X-ray Fluorescence technique (SR-TXRF) was employed to identify and quantify the elements and metals of nutritional and toxicological importance in the wood samples. The analysis was performed in the Brazilian Synchrotron Light Source Laboratory, using a white beam for excitation and a Si(Li) detector for X-ray detection. In several samples, P, K, Ca, Ti, Fe, Sr, Ba and Pb were quantified. The K/Ca, K/P and Pb/Ca ratios were found to decrease towards the bark.

  17. Optimizing total reflection X-ray fluorescence for direct trace element quantification in proteins I: Influence of sample homogeneity and reflector type

    Science.gov (United States)

    Wellenreuther, G.; Fittschen, U. E. A.; Achard, M. E. S.; Faust, A.; Kreplin, X.; Meyer-Klaucke, W.

    2008-12-01

    Total reflection X-ray fluorescence (TXRF) is a very promising method for the direct, quick and reliable multi-elemental quantification of trace elements in protein samples. With the introduction of an internal standard consisting of two reference elements, scandium and gallium, a wide range of proteins can be analyzed, regardless of their salt content, buffer composition, additives and amino acid composition. This strategy also enables quantification of matrix effects. Two potential issues associated with drying have been considered in this study: (1) Formation of heterogeneous residues of varying thickness and/or density; and (2) separation of the internal standard and protein during drying (which has to be prevented to allow accurate quantification). These issues were investigated by microbeam X-ray fluorescence (μXRF) with special emphasis on (I) the influence of sample support and (II) the protein / buffer system used. In the first part, a model protein was studied on well established sample supports used in TXRF, PIXE and XRF (Mylar, siliconized quartz, Plexiglas and silicon). In the second part we imaged proteins of different molecular weight, oligomerization state, bound metals and solubility. A partial separation of protein and internal standard was only observed with untreated silicon, suggesting it may not be an adequate support material. Siliconized quartz proved to be the least prone to heterogeneous drying of the sample and yielded the most reliable results.

  18. Monitoring of the environmental pollution by trace element analysis in tree-rings using synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Sirito de Vives, Ana Elisa; Moreira, Silvana; Brienza, Sandra Maria Boscolo; Silva Medeiros, Jean Gabriel; Tomazello Filho, Mario Tomazello; Araujo Domingues Zucchi, Orgheda Luiza; Nascimento Filho, Virgilio Franco do

    2006-01-01

    This paper aims to study the environmental pollution in the tree development, in order to evaluate its use as bioindicator in urban and country sides. The sample collection was carried out in Piracicaba city, Sao Paulo State, which presents high level of environmental contamination in water, soil and air, due to industrial activities, vehicles combustion, sugar-cane leaves burning in the harvesting, etc. The species Caesalpinia peltophoroides ('Sibipiruna') was selected because it is widely used in urban forestation. Synchrotron Radiation Total Reflection X-ray Fluorescence technique (SR-TXRF) was employed to identify and quantify the elements and metals of nutritional and toxicological importance in the wood samples. The analysis was performed in the Brazilian Synchrotron Light Source Laboratory, using a white beam for excitation and a Si(Li) detector for X-ray detection. In several samples, P, K, Ca, Ti, Fe, Sr, Ba and Pb were quantified. The K/Ca, K/P and Pb/Ca ratios were found to decrease towards the bark

  19. Optimizing total reflection X-ray fluorescence for direct trace element quantification in proteins I: Influence of sample homogeneity and reflector type

    Energy Technology Data Exchange (ETDEWEB)

    Wellenreuther, G. [European Molecular Biology Laboratory, Notkestr. 85, 22603 Hamburg (Germany); Fittschen, U.E.A. [Department of Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Achard, M.E.S.; Faust, A.; Kreplin, X. [European Molecular Biology Laboratory, Notkestr. 85, 22603 Hamburg (Germany); Meyer-Klaucke, W. [European Molecular Biology Laboratory, Notkestr. 85, 22603 Hamburg (Germany)], E-mail: Wolfram@embl-hamburg.de

    2008-12-15

    Total reflection X-ray fluorescence (TXRF) is a very promising method for the direct, quick and reliable multi-elemental quantification of trace elements in protein samples. With the introduction of an internal standard consisting of two reference elements, scandium and gallium, a wide range of proteins can be analyzed, regardless of their salt content, buffer composition, additives and amino acid composition. This strategy also enables quantification of matrix effects. Two potential issues associated with drying have been considered in this study: (1) Formation of heterogeneous residues of varying thickness and/or density; and (2) separation of the internal standard and protein during drying (which has to be prevented to allow accurate quantification). These issues were investigated by microbeam X-ray fluorescence ({mu}XRF) with special emphasis on (I) the influence of sample support and (II) the protein / buffer system used. In the first part, a model protein was studied on well established sample supports used in TXRF, PIXE and XRF (Mylar, siliconized quartz, Plexiglas and silicon). In the second part we imaged proteins of different molecular weight, oligomerization state, bound metals and solubility. A partial separation of protein and internal standard was only observed with untreated silicon, suggesting it may not be an adequate support material. Siliconized quartz proved to be the least prone to heterogeneous drying of the sample and yielded the most reliable results.

  20. Efficient isotope ratio analysis of uranium particles in swipe samples by total-reflection x-ray fluorescence spectrometry and secondary ion mass spectrometry

    International Nuclear Information System (INIS)

    Esaka, Fumitaka; Watanabe, Kazuo; Fukuyama, Hiroyasu; Onodera, Takashi; Esaka, Konomi T.; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu

    2004-01-01

    A new particle recovery method and a sensitive screening method were developed for subsequent isotope ratio analysis of uranium particles in safeguards swipe samples. The particles in the swipe sample were recovered onto a carrier by means of vacuum suction-impact collection method. When grease coating was applied to the carrier, the recovery efficiency was improved to 48±9%, which is superior to that of conventionally-used ultrasoneration method. Prior to isotope ratio analysis with secondary ion mass spectrometry (SIMS), total reflection X-ray fluorescence spectrometry (TXRF) was applied to screen the sample for the presence of uranium particles. By the use of Si carriers in TXRF analysis, the detection limit of 22 pg was achieved for uranium. By combining these methods with SIMS, the isotope ratios of 235 U/ 238 U for individual uranium particles were efficiently determined. (author)

  1. Application of the total reflection X-ray fluorescence method to the elemental analysis of brain tumors of different types and grades of malignancy

    International Nuclear Information System (INIS)

    Lankosz, M.W.; Grzelak, M.; Ostachowicz, B.; Wandzilak, A.; Szczerbowska-Boruchowska, M.; Wrobel, P.; Radwanska, E.; Adamek, D.

    2014-01-01

    The process of carcinogenesis may influence normal biochemical reactions leading to alterations in the elemental composition of the tissue. Total reflection X-ray fluorescence analysis (TXRF) was applied to the elemental analysis of different brain tumors. The following elements were present in all the neoplastic tissues analyzed: K, Ca, Fe, Cu, Zn and Rb. The results of the analysis showed that the elemental composition of a relatively small fragment of tissue represents satisfactorily the biochemical “signature” of a cancer. On the basis of the element concentrations determined, it was possible to differentiate between some types of brain tumors. - Highlights: • Elemental composition represents the biochemical signature of brain cancer. • The element levels differentiate some types of brain tumors. • TXRF spectrometry is a useful tool for elemental trace analysis of brain cancer

  2. Portable ultrahigh-vacuum sample storage system for polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Yoshihide, E-mail: e0827@mosk.tytlabs.co.jp; Nishimura, Yusaku F.; Suzuki, Ryo; Beniya, Atsushi; Isomura, Noritake [Toyota Central R& D Labs., Inc., Yokomichi 41-1, Nagakute, Aichi 480-1192 (Japan); Uehara, Hiromitsu; Asakura, Kiyotaka; Takakusagi, Satoru [Catalysis Research Center, Hokkaido University, Kita 21-10, Sapporo, Hokkaido 001-0021 (Japan); Nimura, Tomoyuki [AVC Co., Ltd., Inada 1450-6, Hitachinaka, Ibaraki 312-0061 (Japan)

    2016-03-15

    A portable ultrahigh-vacuum sample storage system was designed and built to investigate the detailed geometric structures of mass-selected metal clusters on oxide substrates by polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy (PTRF-XAFS). This ultrahigh-vacuum (UHV) sample storage system provides the handover of samples between two different sample manipulating systems. The sample storage system is adaptable for public transportation, facilitating experiments using air-sensitive samples in synchrotron radiation or other quantum beam facilities. The samples were transferred by the developed portable UHV transfer system via a public transportation at a distance over 400 km. The performance of the transfer system was demonstrated by a successful PTRF-XAFS study of Pt{sub 4} clusters deposited on a TiO{sub 2}(110) surface.

  3. Wave-optical evaluation of interference fringes and wavefront phase in a hard-x-ray beam totally reflected by mirror optics.

    Science.gov (United States)

    Yamauchi, Kazuto; Yamamura, Kazuya; Mimura, Hidekazu; Sano, Yasuhisa; Saito, Akira; Endo, Katsuyoshi; Souvorov, Alexei; Yabashi, Makina; Tamasaku, Kenji; Ishikawa, Tetsuya; Mori, Yuzo

    2005-11-10

    The intensity flatness and wavefront shape in a coherent hard-x-ray beam totally reflected by flat mirrors that have surface bumps modeled by Gaussian functions were investigated by use of a wave-optical simulation code. Simulated results revealed the necessity for peak-to-valley height accuracy of better than 1 nm at a lateral resolution near 0.1 mm to remove high-contrast interference fringes and appreciable wavefront phase errors. Three mirrors that had different surface qualities were tested at the 1 km-long beam line at the SPring-8/Japan Synchrotron Radiation Research Institute. Interference fringes faded when the surface figure was corrected below the subnanometer level to a spatial resolution close to 0.1 mm, as indicated by the simulated results.

  4. Studies and developments for the analysis of products of nuclear reprocessing plants with the help of the X-ray fluorescence analysis on totally reflecting sample holders (TXRF)

    International Nuclear Information System (INIS)

    Diercks, H.; Eggers, I.; Gibau, F.; Haarich, M.; Hastenteufel, S.; Haurand, M.; Knoechel, A.; Salow, H.

    1990-01-01

    Studies with inactive and active simulates of products of nuclear reprocessing plants show the suitability of the X-Ray Fluorescence Analysis on Totally Reflecting Sample Holders (TXRF), to detect the available elements simultaneously by direct measurements of specially prepared thin samples. High dilution enables in the most cases, to avoid working in hot cells and to carry out the analysis in glove boxes. The analysis of uranium products and great amounts of matrix elements containing solutions like LAW and MAW demands the separation of the matrix elements before TXRF measurement. Procedures for this task have been developed. The potential of the new analytical procedure was demonstrated by the analysis of two samples of highly diluted high active wastes. (orig.) With 65 refs., 20 tabs., 81 figs [de

  5. Determination of metals by total reflection X-ray fluorescence and evaluation of toxicity of a river impacted by coal mining in the south of Brazil.

    Science.gov (United States)

    Lattuada, R M; Menezes, C T B; Pavei, P T; Peralba, M C R; Dos Santos, J H Z

    2009-04-30

    Metal (Fe, Mn, Zn, Ni, Cd, and Pb) concentrations in the region of Criciuma (Brazil), a region impacted by coal mining, were determined in water and sediments using total reflection X-ray fluorescence (TXRF) spectroscopy. Samples were collected from the Mãe Luzia River (south Brazil) at five different stations, from the source down to the river mouth (Ararangua estuary). Water and sediment toxicity were also evaluated using bioassays with Daphnia magna as the bioindicator. The metal present in the highest concentrations both in water (1.3-11 mg L(-1)) and in sediments (34-142 mg L(-1)) was iron. Results suggest an influence of coal mining on the aquatic receptors, showing a clear relationship between metal content (mostly Fe) and ecotoxicity.

  6. Use of high-intensity sonication for pre-treatment of biological tissues prior to multielemental analysis by total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    De La Calle, Inmaculada; Costas, Marta; Cabaleiro, Noelia; Lavilla, Isela; Bendicho, Carlos

    2012-01-01

    In this work, two ultrasound-based procedures are developed for sample preparation prior to determination of P, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Se and Sr in biological tissues by total reflection X-ray fluorescence spectrometry. Ultrasound-assisted extraction by means of a cup-horn sonoreactor and ultrasonic-probe slurry sampling were compared with a well-established procedure such as magnetic agitation slurry sampling. For that purpose, seven certified reference materials and different real samples of animal tissue were used. Similar accuracy and precision is obtained with the three sample preparation approaches tried. Limits of detection were dependent on both the sample matrix and the sample pre-treatment used, best values being achieved with ultrasound-assisted extraction. Advantages of ultrasound-assisted extraction include reduced sample handling, decreased contamination risks (neither addition of surfactants nor use of foreign objects inside the extraction vial), simpler background (no solid particles onto the sample carrier) and improved recovery for some elements such as P. A mixture of 10% v/v HNO 3 + 20–40% v/v HCl was suitable for extraction from biological tissues. - Highlights: ► We implement high-intensity sonication for pre-treatment of biological tissues. ► Multielemental analysis is performed by total reflection X-ray spectrometry. ► Ultrasound-based procedures are developed and compared to conventional slurry preparation. ► Features such as background, recovery and sample handling are favored by using ultrasonic extraction.

  7. Room temperature trapping of stibine and bismuthine onto quartz substrates coated with nanostructured palladium for total reflection X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

    2015-05-01

    In this work, a novel method for determining Sb and Bi based on the trapping of their covalent hydrides onto quartz reflectors coated with immobilized palladium nanoparticles (Pd NPs) followed by total reflection X-ray fluorescence (TXRF) analysis is proposed. Pd NPs were synthesized by chemical reduction of the metal precursor using a mixture of water:ethanol as mild reducing agent. Silanization using 3-mercaptopropyltrimethoxysilane (MPTMS) was performed for the immobilization of Pd NPs onto the quartz substrates. Volatile hydrides (stibine and bismuthine) generated by means of a continuous flow system were flushed onto the immobilized Pd NPs and retained by catalytic decomposition. As a result of the high catalytic activity of the nanostructured film, trapping can be performed at ambient temperature with good efficiency. Limits of detection (LODs) were 2.3 and 0.70 μg L{sup −1} for Sb and Bi, respectively. Enrichment factors of 534 and 192 were obtained for Sb and Bi, respectively. The new method was applied for the analysis of several matrices (milk, soil, sediment, cutaneous powder). Recoveries were in the range of 98.4–101% for both elements with a relative standard deviation of 2.5% (N = 5). - Highlights: • A novel method for trapping covalent hydrides of antimony and bismuth is proposed. • Emphasis is placed on the application of Pd nanoparticles as trapping surface. • The nanostructured surface provides high catalytic activity at ambient temperature. • Analysis by total reflection X-ray fluorescence is performed. • Determination of Bi and Sb in different matrices is carried out.

  8. Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

    International Nuclear Information System (INIS)

    Stosnach, Hagen; Mages, Margarete

    2009-01-01

    In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

  9. Total reflection X-ray fluorescence spectrometric determination of elements in water hyacinth from the Lerma River

    Energy Technology Data Exchange (ETDEWEB)

    Tejeda, S. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Instituto Tecnologico de Toluca, Division de Estudios de Posgrado e Investigacion, Apartado Postal 890, Metepec, C.P. 52149 (Mexico); Zarazua, G., E-mail: graciela.zarazua@inin.gob.m [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Avila-Perez, P. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Instituto Tecnologico de Toluca, Division de Estudios de Posgrado e Investigacion, Apartado Postal 890, Metepec, C.P. 52149 (Mexico); Carapia-Morales, L. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Martinez, T. [Universidad Nacional Autonoma de Mexico, Facultad de Quimica, Mexico D.F. (Mexico)

    2010-06-15

    The Lerma River is one of the most polluted body water in Mexico. For this reason, only the highly resistant organisms such as water hyacinth are able to reproduce in this river. The aim of this work was to evaluate the concentration of K, S, Fe, Ca, Mn, Ti, Zn, Sr, Rb, Cu, Cr, Ni, Pb and Br in roots of water hyacinth (Eichhornia crassipes) from the Lerma River. The samples were collected from five sites in the river and analyzed in triplicate using a TXRF Spectrometer 'TX-2000 Ital Structures' with a Si(Li) detector and a resolution of 140 eV (FWHM) at Mn K{alpha}. A Mo tube (40 kV, 30 mA) with 17.4 KeV excitation energy was used for a counting time of 500 s. Results show that the average metal concentration in the water hyacinth roots decrease in the following order: K (9698.2 {mu}g/g) > S (7593.3 {mu}g/g) > Fe (4406.6 {mu}g/g) > Ca (2601.8 {mu}g/g) > Mn (604.2 {mu}g/g) > Ti (230.7 {mu}g/g) > Zn (51.65 {mu}g/g) > Sr (43.55 {mu}g/g) > Rb (18.61 {mu}g/g) > Cu (12.78 {mu}g/g) > Cr (6.45 {mu}g/g) > Ni (4.68 {mu}g/g) > Pb (4.32 {mu}g/g) > Br (4.31 {mu}g/g) and the bioconcentration factors in the water hyacinth decrease in the sequence: Ti > Fe > Mn > Cu > Ni > Zn > S > Pb > Rb > K > Cr > Sr > Br > Ca. The concentrations in roots of water hyacinth reflect the high pollution level of the river.

  10. Total reflection X-ray fluorescence spectrometric determination of elements in water hyacinth from the Lerma River

    Science.gov (United States)

    Tejeda, S.; Zarazúa, G.; Ávila-Pérez, P.; Carapia-Morales, L.; Martínez, T.

    2010-06-01

    The Lerma River is one of the most polluted body water in Mexico. For this reason, only the highly resistant organisms such as water hyacinth are able to reproduce in this river. The aim of this work was to evaluate the concentration of K, S, Fe, Ca, Mn, Ti, Zn, Sr, Rb, Cu, Cr, Ni, Pb and Br in roots of water hyacinth ( Eichhornia crassipes) from the Lerma River. The samples were collected from five sites in the river and analyzed in triplicate using a TXRF Spectrometer 'TX-2000 Ital Structures' with a Si(Li) detector and a resolution of 140 eV (FWHM) at Mn Kα. A Mo tube (40 kV, 30 mA) with 17.4 KeV excitation energy was used for a counting time of 500 s. Results show that the average metal concentration in the water hyacinth roots decrease in the following order: K (9698.2 µg/g) > S (7593.3 µg/g) > Fe (4406.6 µg/g) > Ca (2601.8 µg/g) > Mn (604.2 µg/g) > Ti (230.7 µg/g) > Zn (51.65 µg/g) > Sr (43.55 µg/g) > Rb (18.61 µg/g) > Cu (12.78 µg/g) > Cr (6.45 µg/g) > Ni (4.68 µg/g) > Pb (4.32 µg/g) > Br (4.31 µg/g) and the bioconcentration factors in the water hyacinth decrease in the sequence: Ti > Fe > Mn > Cu > Ni > Zn > S > Pb > Rb > K > Cr > Sr > Br > Ca. The concentrations in roots of water hyacinth reflect the high pollution level of the river.

  11. Total reflection X-ray fluorescence spectrometric determination of elements in water hyacinth from the Lerma River

    International Nuclear Information System (INIS)

    Tejeda, S.; Zarazua, G.; Avila-Perez, P.; Carapia-Morales, L.; Martinez, T.

    2010-01-01

    The Lerma River is one of the most polluted body water in Mexico. For this reason, only the highly resistant organisms such as water hyacinth are able to reproduce in this river. The aim of this work was to evaluate the concentration of K, S, Fe, Ca, Mn, Ti, Zn, Sr, Rb, Cu, Cr, Ni, Pb and Br in roots of water hyacinth (Eichhornia crassipes) from the Lerma River. The samples were collected from five sites in the river and analyzed in triplicate using a TXRF Spectrometer 'TX-2000 Ital Structures' with a Si(Li) detector and a resolution of 140 eV (FWHM) at Mn Kα. A Mo tube (40 kV, 30 mA) with 17.4 KeV excitation energy was used for a counting time of 500 s. Results show that the average metal concentration in the water hyacinth roots decrease in the following order: K (9698.2 μg/g) > S (7593.3 μg/g) > Fe (4406.6 μg/g) > Ca (2601.8 μg/g) > Mn (604.2 μg/g) > Ti (230.7 μg/g) > Zn (51.65 μg/g) > Sr (43.55 μg/g) > Rb (18.61 μg/g) > Cu (12.78 μg/g) > Cr (6.45 μg/g) > Ni (4.68 μg/g) > Pb (4.32 μg/g) > Br (4.31 μg/g) and the bioconcentration factors in the water hyacinth decrease in the sequence: Ti > Fe > Mn > Cu > Ni > Zn > S > Pb > Rb > K > Cr > Sr > Br > Ca. The concentrations in roots of water hyacinth reflect the high pollution level of the river.

  12. X-ray reflection in oxygen-rich accretion discs of ultracompact X-ray binaries

    DEFF Research Database (Denmark)

    Madej, O. K.; Garcia, Jeronimo; Jonker, P. G.

    2014-01-01

    We present spectroscopic X-ray data of two candidate ultracompact X-ray binaries (UCXBs): 4U 0614+091 and 4U 1543-624. We confirm the presence of a broad O viii Ly alpha reflection line (at a parts per thousand 18 angstrom) using XMM-Newton and Chandra observations obtained in 2012 and 2013. The ...

  13. Speciation of copper and zinc in size-fractionated atmospheric particulate matter using total reflection mode X-ray absorption near-edge structure spectrometry

    International Nuclear Information System (INIS)

    Osan, Janos; Meirer, Florian; Groma, Veronika; Toeroek, Szabina; Ingerle, Dieter; Streli, Christina; Pepponi, Giancarlo

    2010-01-01

    The health effects of aerosol depend on the size distribution and the chemical composition of the particles. Heavy metals of anthropogenic origin are bound to the fine aerosol fraction (PM 2.5 ). The composition and speciation of aerosol particles can be variable in time, due to the time-dependence of anthropogenic sources as well as meteorological conditions. Synchrotron-radiation total reflection X-ray fluorescence (SR-TXRF) provides very high sensitivity for characterization of atmospheric particulate matter. X-ray absorption near-edge structure (XANES) spectrometry in conjunction with TXRF detection can deliver speciation information on heavy metals in aerosol particles collected directly on the reflector surface. The suitability of TXRF-XANES for copper and zinc speciation in size-fractionated atmospheric particulate matter from a short sampling period is presented. For high size resolution analysis, atmospheric aerosol particles were collected at different urban and rural locations using a 7-stage May cascade impactor having adapted for sampling on Si wafers. The thin stripe geometry formed by the particulate matter deposited on the May-impactor plates is ideally suited to SR-TXRF. Capabilities of the combination of the May-impactor sampling and TXRF-XANES measurements at HASYLAB Beamline L to Cu and Zn speciation in size-fractionated atmospheric particulate matter are demonstrated. Information on Cu and Zn speciation could be performed for elemental concentrations as low as 140 pg/m 3 . The Cu and Zn speciation in the different size fraction was found to be very distinctive for samples of different origin. Zn and Cu chemical state typical for soils was detected only in the largest particles studied (2-4 μm fraction). The fine particles, however, contained the metals of interest in the sulfate and nitrate forms.

  14. Multielement analysis of swiss mice brains with Alzheimer's disease induced by beta amyloid oligomers using a portable total reflection X-ray fluorescence system

    International Nuclear Information System (INIS)

    Almeida, Danielle S.; Brigido, Matheus M.; Anjos, Marcelino J.; Ferreira, Sergio S.; Souza, Amanda S.; Lopes, Ricardo T.

    2017-01-01

    Alzheimer's disease (AD) is a progressive dementia that, in early stages, manifests as a profound inability to form new memories. The pathological features of AD include β-amyloid (Aβ) plaques, intracellular neurofibrillary tangles, loss of neurons and synapses, and activation of glia cells. Recently, several groups have raised the 'metal hypothesis' of AD. Metal ions, such as Cu and Zn, have been demonstrated to modulate amyloid aggregation along different pathways. Extensive research has been conducted on the effects of metals on Aβ aggregation and all of them have shown that both Cu and Zn accelerate the aggregation by shortening, or eliminating, the lag phase associated with the amyloid fibrillation process. The metal ions mentioned previously may have an important impact on the protein misfolding and the progression of the neurodegenerative process. The TXRF technique is very important, because can be used to identify and quantify trace elements present in the sample at very low concentrations (μg.g"-"1). In this work, three groups of females were studied: control, AD10 and AD100. The groups AD10 and AD100 were given a single intracerebroventricular injection of 10 pmol and 100 pmol of oligomers of β-amyloid peptide respectively to be induced AD. The TXRF measurements were performed using a portable total reflection X-ray fluorescence system developed in the Laboratory of Nuclear Instrumentation (LIN/UFRJ) that uses an X-ray tube with a molybdenum anode operating at 40 kV and 500 mA used for the excitation and a detector Si-PIN with energy resolution of 145 eV at 200 eV. It was possible to determine the concentrations of the following elements: P, S, K, Fe, Cu, Zn and Rubidium. Results showed differences in the elemental concentration in some brain regions between the AD groups and the control group. (author)

  15. Evaluation of growth tree rings of Tipuana Tipu as biomonitoring of environmental pollution by synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Moreira, Silvana; Geraldo, Simoni Michetti; Canteras, Felippe Benavente

    2013-01-01

    The bioindicators, plants or animals capable to present qualitative and/or quantitative answers, when exposed to pollutant substances. Trees record and incorporate in their log, developed year after year, the impressions of the environment, becoming possible the study of the different environmental changes, including contamination, that have occurred over the life of these trees. The selected species, Tipuana Tipu, of the Leguminosae family, is native of Argentina and Bolivia and was introduced in Brazil as an ornamental plant. It is one of the most common trees in the urban landscaping in Sao Paulo city. The present project has as main objective the determination of the content of potentially toxic elements in samples of growth the tree rings of Tipuana Tipu, previously dated, collected in strategically locations of Sao Paulo, using Synchrotron Radiation Total Reflection X-Ray Fluorescence. Samples were also collected in the Piracicaba (SP), local of little access and small flow traffic. The SR-TXRF analysis was carried out in the X-ray Fluorescence Beamline at the Brazilian Synchrotron Light Source Laboratory, located in Campinas city, Sao Paulo State, Brazil. Some trace elements present concentrations higher than considered as normal in some periods. In this paper the highest value for Pb was 123.54 μg.g -1 considered as threshold value was observed for the period 1998 to 2000 for University of Sao Paulo, Butanta site. For the same period excessive level was also observed for samples collected in Piracicaba city. In Sao Paulo city, sample collected in the campus of University of Sao Paulo (Butanta), showed the highest toxicity, with concentration above the tolerable limit for Ti, Cr and Cu. For the samples collected in Piracicaba city the concentrations of Cr, Ni, Cu, and Pb exceeding the toxicity limits. (author)

  16. Evaluation of growth tree rings of Tipuana Tipu as biomonitoring of environmental pollution by synchrotron radiation total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Geraldo, Simoni Michetti; Canteras, Felippe Benavente, E-mail: silvana@fec.unicamp.br, E-mail: felippe.canteras@gmail.com [Universidade Estadual de Campinas (FEC/UNICAMP), Campinas, SP (Brazil). Dept. de Saneamento e Ambiente

    2013-07-01

    The bioindicators, plants or animals capable to present qualitative and/or quantitative answers, when exposed to pollutant substances. Trees record and incorporate in their log, developed year after year, the impressions of the environment, becoming possible the study of the different environmental changes, including contamination, that have occurred over the life of these trees. The selected species, Tipuana Tipu, of the Leguminosae family, is native of Argentina and Bolivia and was introduced in Brazil as an ornamental plant. It is one of the most common trees in the urban landscaping in Sao Paulo city. The present project has as main objective the determination of the content of potentially toxic elements in samples of growth the tree rings of Tipuana Tipu, previously dated, collected in strategically locations of Sao Paulo, using Synchrotron Radiation Total Reflection X-Ray Fluorescence. Samples were also collected in the Piracicaba (SP), local of little access and small flow traffic. The SR-TXRF analysis was carried out in the X-ray Fluorescence Beamline at the Brazilian Synchrotron Light Source Laboratory, located in Campinas city, Sao Paulo State, Brazil. Some trace elements present concentrations higher than considered as normal in some periods. In this paper the highest value for Pb was 123.54 μg.g{sup -1} considered as threshold value was observed for the period 1998 to 2000 for University of Sao Paulo, Butanta site. For the same period excessive level was also observed for samples collected in Piracicaba city. In Sao Paulo city, sample collected in the campus of University of Sao Paulo (Butanta), showed the highest toxicity, with concentration above the tolerable limit for Ti, Cr and Cu. For the samples collected in Piracicaba city the concentrations of Cr, Ni, Cu, and Pb exceeding the toxicity limits. (author)

  17. Development of Total Reflection X-ray fluorescence spectrometry quantitative methodologies for elemental characterization of building materials and their degradation products

    Science.gov (United States)

    García-Florentino, Cristina; Maguregui, Maite; Marguí, Eva; Torrent, Laura; Queralt, Ignasi; Madariaga, Juan Manuel

    2018-05-01

    In this work, a Total Reflection X-ray fluorescence (TXRF) spectrometry based quantitative methodology for elemental characterization of liquid extracts and solids belonging to old building materials and their degradation products from a building of the beginning of 20th century with a high historic cultural value in Getxo, (Basque Country, North of Spain) is proposed. This quantification strategy can be considered a faster methodology comparing to traditional Energy or Wavelength Dispersive X-ray fluorescence (ED-XRF and WD-XRF) spectrometry based methodologies or other techniques such as Inductively Coupled Plasma Mass Spectrometry (ICP-MS). In particular, two kinds of liquid extracts were analysed: (i) water soluble extracts from different mortars and (ii) acid extracts from mortars, black crusts, and calcium carbonate formations. In order to try to avoid the acid extraction step of the materials and their degradation products, it was also studied the TXRF direct measurement of the powdered solid suspensions in water. With this aim, different parameters such as the deposition volume and the measuring time were studied for each kind of samples. Depending on the quantified element, the limits of detection achieved with the TXRF quantitative methodologies for liquid extracts and solids were set around 0.01-1.2 and 2-200 mg/L respectively. The quantification of K, Ca, Ti, Mn, Fe, Zn, Rb, Sr, Sn and Pb in the liquid extracts was proved to be a faster alternative to other more classic quantification techniques (i.e. ICP-MS), accurate enough to obtain information about the composition of the acidic soluble part of the materials and their degradation products. Regarding the solid samples measured as suspensions, it was quite difficult to obtain stable and repetitive suspensions affecting in this way the accuracy of the results. To cope with this problem, correction factors based on the quantitative results obtained using ED-XRF were calculated to improve the accuracy of

  18. Multielement analysis of swiss mice brains with Alzheimer's disease induced by beta amyloid oligomers using a portable total reflection X-ray fluorescence system

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Danielle S.; Brigido, Matheus M.; Anjos, Marcelino J.; Ferreira, Sergio S.; Souza, Amanda S.; Lopes, Ricardo T., E-mail: ricardo@lin.ufrj.br, E-mail: marcelin@uerj.br, E-mail: amandass@bioqmed.ufrj.br, E-mail: ferreira@bioqmed.ufrj.br, E-mail: amandass@bioqmed.ufrj.br [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil); Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil); Instituto de Fisica Armando Dias Tavares (Brazil)

    2017-11-01

    Alzheimer's disease (AD) is a progressive dementia that, in early stages, manifests as a profound inability to form new memories. The pathological features of AD include β-amyloid (Aβ) plaques, intracellular neurofibrillary tangles, loss of neurons and synapses, and activation of glia cells. Recently, several groups have raised the 'metal hypothesis' of AD. Metal ions, such as Cu and Zn, have been demonstrated to modulate amyloid aggregation along different pathways. Extensive research has been conducted on the effects of metals on Aβ aggregation and all of them have shown that both Cu and Zn accelerate the aggregation by shortening, or eliminating, the lag phase associated with the amyloid fibrillation process. The metal ions mentioned previously may have an important impact on the protein misfolding and the progression of the neurodegenerative process. The TXRF technique is very important, because can be used to identify and quantify trace elements present in the sample at very low concentrations (μg.g{sup -1}). In this work, three groups of females were studied: control, AD10 and AD100. The groups AD10 and AD100 were given a single intracerebroventricular injection of 10 pmol and 100 pmol of oligomers of β-amyloid peptide respectively to be induced AD. The TXRF measurements were performed using a portable total reflection X-ray fluorescence system developed in the Laboratory of Nuclear Instrumentation (LIN/UFRJ) that uses an X-ray tube with a molybdenum anode operating at 40 kV and 500 mA used for the excitation and a detector Si-PIN with energy resolution of 145 eV at 200 eV. It was possible to determine the concentrations of the following elements: P, S, K, Fe, Cu, Zn and Rubidium. Results showed differences in the elemental concentration in some brain regions between the AD groups and the control group. (author)

  19. Evaluation of Fe and Zn/Cu ratio in serum of patients with sickle cell anemia by total reflection X-ray fluorescence using synchrotron radiation

    International Nuclear Information System (INIS)

    Canellas, Catarine G.L.; Leitao, Roberta G.; Lopes, Ricardo T.; Bellido, Alfredo Victor B.; Anjos, Marcelino J.

    2011-01-01

    Sickle cell anemia (SCA) is a blood disorder that affects hemoglobin, the protein found in red blood cells that help carry oxygen throughout the body. In this work we have analyzed serum samples from patients with SCA by using total reflection X-ray fluorescence using synchrotron radiation (SRTXRF). The SRTXRF measurements were performed at the X-ray fluorescence beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, Sao Paulo using a polychromatic beam. We have studied forty-three patients aged 18-50 years old, suffering from SCA and Sixty healthy volunteers aged 18-60 years old. It was possible to determine the concentrations of the following elements: P, S, Cl, K, Ca, Fe, Cu, Zn, Br and Rb. Student's t-test was applied in order to check whether the two populations (CG x SCA) had the same mean values. It was observed that elemental concentration of P, Cl, K, Fe, Cu, Zn and Br differed significantly (α = 0.05) between groups of healthy subjects and SCA. The concentrations of K, Fe and Cu in the serum samples of patients with SCA were larger 15%, 120 % and 20 %, respectively, when compared with the CG. On the other hand, the concentrations of P (-20 %), Cl (-6 %), Zn (-25 %) and Br (-22 %) were smaller than the values determined for the control group. The serum level Cu/Zn ratio was significantly higher (60%) in the serum samples of patients with SCA group than the CG. So, the Cu/Zn ratio can be used as an adjuvant index in enhancement for diagnosis of SCA. There are evidences of an association among Fe, Cu, Zn and Cu/Zn in the SCA pathogenesis process. (author)

  20. Evaluation of Fe and Zn/Cu ratio in serum of patients with sickle cell anemia by total reflection X-ray fluorescence using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Canellas, Catarine G.L.; Leitao, Roberta G.; Lopes, Ricardo T., E-mail: catarine@lin.ufrj.b, E-mail: ricardo@lin.ufrj.b [Universidade Federal do Rio de Janeiro (PEN/COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Programa de Engenharia Nuclear. Lab. de Instrumentaco Nuclear; Carvalho, Silvia M.F., E-mail: silvia@hemorio.rj.gov.b [State Institute of Hematology Arthur de Siqueira Cavalcanti (HEMORIO), Rio de Janeiro, RJ (Brazil); Bellido, Alfredo Victor B., E-mail: alfredo@ien.gov.b [Federal Fluminense University (UFF), Niteroi, RJ (Brazil). Chemistry Inst.; Anjos, Marcelino J., E-mail: marcelin@lin.ufrj.b [State University of Rio de Janeiro (UERJ), RJ (Brazil). Physics Inst.

    2011-07-01

    Sickle cell anemia (SCA) is a blood disorder that affects hemoglobin, the protein found in red blood cells that help carry oxygen throughout the body. In this work we have analyzed serum samples from patients with SCA by using total reflection X-ray fluorescence using synchrotron radiation (SRTXRF). The SRTXRF measurements were performed at the X-ray fluorescence beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, Sao Paulo using a polychromatic beam. We have studied forty-three patients aged 18-50 years old, suffering from SCA and Sixty healthy volunteers aged 18-60 years old. It was possible to determine the concentrations of the following elements: P, S, Cl, K, Ca, Fe, Cu, Zn, Br and Rb. Student's t-test was applied in order to check whether the two populations (CG x SCA) had the same mean values. It was observed that elemental concentration of P, Cl, K, Fe, Cu, Zn and Br differed significantly ({alpha} = 0.05) between groups of healthy subjects and SCA. The concentrations of K, Fe and Cu in the serum samples of patients with SCA were larger 15%, 120 % and 20 %, respectively, when compared with the CG. On the other hand, the concentrations of P (-20 %), Cl (-6 %), Zn (-25 %) and Br (-22 %) were smaller than the values determined for the control group. The serum level Cu/Zn ratio was significantly higher (60%) in the serum samples of patients with SCA group than the CG. So, the Cu/Zn ratio can be used as an adjuvant index in enhancement for diagnosis of SCA. There are evidences of an association among Fe, Cu, Zn and Cu/Zn in the SCA pathogenesis process. (author)

  1. Evaluation of Fe and Zn/Cu ratio in serum of patients with sickle cell anemia by total reflection X-ray fluorescence using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Canellas, Catarine G.L.; Leitao, Roberta G; Lopes, Ricardo T., E-mail: catarine@lin.ufrj.b, E-mail: ricardo@lin.ufrj.b [Universidade Federal do Rio de Janeiro (PEN/COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Programa de Engenharia Nuclear. Lab. de Instrumentaco Nuclear; Carvalho, Silvia M.F., E-mail: silvia@hemorio.rj.gov.b [State Institute of Hematology Arthur de Siqueira Cavalcanti (HEMORIO), Rio de Janeiro, RJ (Brazil); Bellido, Alfredo Victor B., E-mail: alfredo@ien.gov.b [Federal Fluminense University (UFF), Niteroi, RJ (Brazil). Chemistry Inst.; Anjos, Marcelino J., E-mail: marcelin@lin.ufrj.b [State University of Rio de Janeiro (UERJ), RJ (Brazil). Physics Inst.

    2011-07-01

    Sickle cell anemia (SCA) is a blood disorder that affects hemoglobin, the protein found in red blood cells that help carry oxygen throughout the body. In this work we have analyzed serum samples from patients with SCA by using total reflection X-ray fluorescence using synchrotron radiation (SRTXRF). The SRTXRF measurements were performed at the X-ray fluorescence beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, Sao Paulo using a polychromatic beam. We have studied forty-three patients aged 18-50 years old, suffering from SCA and Sixty healthy volunteers aged 18-60 years old. It was possible to determine the concentrations of the following elements: P, S, Cl, K, Ca, Fe, Cu, Zn, Br and Rb. Student's t-test was applied in order to check whether the two populations (CG x SCA) had the same mean values. It was observed that elemental concentration of P, Cl, K, Fe, Cu, Zn and Br differed significantly ({alpha} = 0.05) between groups of healthy subjects and SCA. The concentrations of K, Fe and Cu in the serum samples of patients with SCA were larger 15%, 120 % and 20 %, respectively, when compared with the CG. On the other hand, the concentrations of P (-20 %), Cl (-6 %), Zn (-25 %) and Br (-22 %) were smaller than the values determined for the control group. The serum level Cu/Zn ratio was significantly higher (60%) in the serum samples of patients with SCA group than the CG. So, the Cu/Zn ratio can be used as an adjuvant index in enhancement for diagnosis of SCA. There are evidences of an association among Fe, Cu, Zn and Cu/Zn in the SCA pathogenesis process. (author)

  2. Trace element analysis of mineral and tap water samples using total reflection x-ray fluorescence (TXRF)

    International Nuclear Information System (INIS)

    Mangala, M.J.; Korir, K.A.; Maina, D.M.; Kinyua, A.M.

    2000-01-01

    Results of trace element analysis by TXRF of tap water and various brands of bottled mineral water samples which are representative of local and imported brands sold in Nairobi are reported. The variation in elemental concentrations in water samples analyzed were as follows: potassium (K) 0.2 to 28.9 μg/ml; calcium (Ca) 2.2 to 120 μg/ml; titanium (Ti) 11 to 60 μg/l; manganese (Mn) 8 to 670 μg/l; iron (Fe) 31 to 540 μg/l; copper (Cu) 8 to 30 μg/l; zinc (Zn) 8 to 4730 μg/l; bromine (Br) 9 to 248 μg/l; rubidium (Rb) 10 to 40 μg/l and strontium (Sr) 10 to 1000 μg/l. Local mineral water samples contain higher levels of trace elements; manganese (Mn), zinc (Zn), bromine (Br), rubidium (Rb) and strontium (Sr) as compared to the imported brands. Principal component analysis of the results revealed three component loading factors clusters for: rubidium (Rb), strontium (Sr) and calcium (Ca); titanium (Ti), iron (Fe), bromine (Br), and zinc (Zn); zinc (Zn), manganese (Mn) and potassium (K) respectively. The percentage of total variance explained by the components was 31.4, 27.3, and 14.8 respectively. In this study, we also found that a limited spread of 5-6 mm for a 10 μl sample was achieved when the quartz sample carrier was dried in a low pressure (300 mbar) oven at 70 o C for 10 hours. (author)

  3. Biomonitoring of environmental pollution using growth tree rings of Tipuana tipu: Quantification by synchrotron radiation total reflection X-ray fluorescence

    Science.gov (United States)

    Geraldo, S. M.; Canteras, F. B.; Moreira, S.

    2014-02-01

    Currently, many studies use the bioindicators to qualitatively and/or quantitatively measure pollution. The analyses of tree growth rings represent one such bioindicator as changes in the environment are often recorded as impressions in the wood. The main objective of the present study is to examine the growth rings of Tipuana tipu - a member of the Leguminosae family that is native to Argentina and Bolivia and was introduced in Brazil as an ornamental plant - for potentially toxic elements. T. tipu is one of the most common trees in the urban landscape of Sao Paulo city and would provide an accurate reflection of environment changes. Tree ring samples previously dated using Synchrotron Radiation Total Reflection X-ray Fluorescence were collected from strategic locations in Sao Paulo. These locations include Piracicaba (SP) that has little access and small flow traffic and the campus of the University of São Paulo. Some trace elements present concentrations higher than considered as normal in some periods. In São Paulo city, samples collected from the campus of University of São Paulo (Butantã), showed the highest toxicity, with concentrations above the tolerable limit for the elements: Cr, Cu, and Pb. For the samples collected in Piracicaba city, one sample presented highest concentrations for the majority of the elements when compared to the other four samples collected at the same place, exceeding the toxicity limits for: Cr, Ni, Cu, and Pb.

  4. Seasonal determination of trace and ultra-trace content in Macrocystis pyrifera from San Jorge Gulf (Patagonia) by Total Reflection X-ray Fluorescence

    Science.gov (United States)

    Salomone, Vanesa N.; Riera, Marina; Cerchietti, Luciana; Custo, Graciela; Muniain, Claudia

    2017-05-01

    Seaweed have a great capacity to accumulate heavy metals in their tissues. The chemical characterization of seaweed is important due to their use in environmental monitoring and human or animal food. The aim of the present study was to evaluate the multi-elemental composition of seaweed from San Jorge Gulf (Patagonia, Argentina) by Total Reflection X-ray Fluorescence (TXRF). The elements As, Br, Cu, Cr, Fe, Mn, Ni, Pb, Rb, Sr, V and Zn were seasonally analyzed and quantified in blades of Macrocystis pyrifera. TXRF showed to be a suitable technique for simultaneous multi-element analysis in this kind of samples. The results revealed seasonal variations in the chemical content for some elements; arsenic content was maximum in summer and autumn, iron concentration increased to the winter and zinc concentration was maximum in autumn. The sum of principal micronutrients (Fe + Zn + Mn + Cu) varied between 114 and 171 mg k- 1 g dw. The total As concentration ranged between 36 and 66 mg kg- 1. Lead, nickel and copper were not detected.

  5. Biofilms as bio-indicator for polluted waters? Total reflection X-ray fluorescence analysis of biofilms of the Tisza river (Hungary)

    Energy Technology Data Exchange (ETDEWEB)

    Mages, Margarete; Ovari, Mihaly; Tuempling, Wolf v. [Department of Inland Water Research Magdeburg, UFZ Centre for Environmental Research Leipzig-Halle, Brueckstrasse 3a, 39114, Magdeburg (Germany); Kroepfl, Krisztina [Department of Chemical Technology and Environmental Chemistry, Eoetvoes University, Pazmany Peter setany 1/A, 1117, Budapest (Hungary)

    2004-02-01

    The aim of this work was to investigate the heavy metal accumulation by natural biofilms living in the catchment area of the Tisza river in Hungary, as well as in biofilms cultivated in vitro. Laboratory tests have demonstrated that metals can be adsorbed on biofilms, depending on their concentration and on the availability of free sorptive places. Biofilms were cultivated in vitro in natural freshwater from the Saale river, Germany. After reaching the plateau phase, Cu was added to reach a concentration of 100 {mu}g/L. An increase of its mass fraction in the biofilm was observed, which caused the decrease of the concentration in the water phase. Unfortunately, the reactor wall was also found to act as adsorbent for Cu. More detailed results of our in vitro experiments will be published in a forthcoming paper. Naturally grown biofilm samples from exposed as well as background places at the Hungarian rivers Szamos and Tisza were collected in 2000 and 2002 after the cyanide spill, and analysed using total reflection X-ray fluorescence analysis (TXRF). Metal mass fraction differences as high as two orders of magnitude were found between polluted and unpolluted (background) sampling points. Extremely high concentration values, e.g. 5600 {mu}g/g Zn in biofilm, were found at highly polluted sampling points. This means an enrichment factor of ca. 10,000 compared to the water phase. (orig.)

  6. Total reflection X-ray fluorescence measurements of S and P in proteins using a vacuum chamber specially designed for low Z elements

    International Nuclear Information System (INIS)

    Rauwolf, M.; Vanhoof, C.; Tirez, K.; Maes, E.; Ingerle, D.; Wobrauschek, P.; Streli, C.

    2014-01-01

    As the ratio of phosphorus and sulfur in proteins allows the determination of the phosphorylation degree in proteins, the absolute determination of phosphorus and sulfur in organic samples is of growing interest. While it takes some effort to quantify phosphorus and sulfur with inductively coupled quadrupole plasma mass spectrometry (ICP-QMS), total reflection X-ray fluorescence analysis (TXRF) allows easy quantification. In the presented work, the low Z TXRF spectrometer at the Atominstitut was used to analyze phosphorus and sulfur in proteins. Although the preparation of the protein samples proved to be more difficult than originally expected, it could be shown that TXRF is well suited for the determination of P and S in proteins. The obtained lower limits of detection (LLD) for P and S in proteins were extrapolated for 1000s and were 34 pg and 19 pg, respectively. The importance of height scans for each sample to exclude heterogeneities was demonstrated. - Highlights: • Low Z TXRF spectrometry was used to analyze phosphorus and sulfur in proteins. • TXRF is well suited for the determination of P and S in proteins. • Good detection limits for P (34 pg) and S (19 pg) were achieved. • Due to the detection limits, we propose that TXRF is a suitable method to analyze protein fractions

  7. Effect of modulation of the particle size distributions in the direct solid analysis by total-reflection X-ray fluorescence

    Science.gov (United States)

    Fernández-Ruiz, Ramón; Friedrich K., E. Josue; Redrejo, M. J.

    2018-02-01

    The main goal of this work was to investigate, in a systematic way, the influence of the controlled modulation of the particle size distribution of a representative solid sample with respect to the more relevant analytical parameters of the Direct Solid Analysis (DSA) by Total-reflection X-Ray Fluorescence (TXRF) quantitative method. In particular, accuracy, uncertainty, linearity and detection limits were correlated with the main parameters of their size distributions for the following elements; Al, Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Ba and Pb. In all cases strong correlations were finded. The main conclusion of this work can be resumed as follows; the modulation of particles shape to lower average sizes next to a minimization of the width of particle size distributions, produce a strong increment of accuracy, minimization of uncertainties and limit of detections for DSA-TXRF methodology. These achievements allow the future use of the DSA-TXRF analytical methodology for development of ISO norms and standardized protocols for the direct analysis of solids by mean of TXRF.

  8. Multielement analysis of environmental samples by total-reflection X-ray fluorescence sprectrometry, neutron activation analysis and inductively coupled plasma optical emission spectroscopy

    International Nuclear Information System (INIS)

    Michaelis, W.

    1986-01-01

    In environmental research and protection trace elements have to be determined over a wide range of atomic number, down to very low concentrations, and in quite different matrices. This challenge requires the availability of complementary analytical methods characterized by a high detection power and few sources of systematic errors. Besides, the capacity of multielement detection is often desired since it facilitates the talking of many problems in which numerous trace elements are of direct concern. Total-reflection X-ray fluorescence, neutron activation analysis and inductively coupled plasma optical emission spectroscopy, in principle fulfill these requirements quite well. However, each method has its domain, and the application to certain sample species may be less promising. Under this aspect, the paper summarizes some recent developments and investigations, including intercomparisons as far as possible. Various matrices are considered : rainwater and airborne particulates, soil samples, river sediments and suspended particulate matter, river water filtrates, ozean water, and organic matrices. Capabilities and limitations are discussed. Sample preparation techniques are described if they are new or essential for achieving the results given. (orig.) [de

  9. Quantification of potentially toxic elements in sewage and sludge from treatment plants in the cities of Campinas and Jaguariuna using synchrotron radiation total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Luciana Carla Ferreira de; Canteras, Felippe Benavente; Moreira, Silvana, E-mail: silvana@fec.unicamp.br, E-mail: felippe.canteras@gmail.com, E-mail: lucarla24@gmail.com [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil). Inst. Politecnico. Dept. de Saneamento e Ambiente

    2013-07-01

    The rapid urban and industrial development in last decades has brought as one of the consequences, changes in the environment. The lack of planning of city growth is, today, one of the major causes of water pollution including residential, industrial, agricultural, and hospital waste. The metals contamination is a major problem, causing serious changes to the environment, causing harm to human health. The sludge generated at sewage treatment plants, is an important source of nutrients and organic matter, and therefore it can also be reused mainly for agricultural use, since contaminants are removed. The cities of Campinas and Jaguariuna are inserted in the Campinas Metropolitan Region (CMR), one of the most dynamic regions in the Brazilian economy. Therefore, to study the anthropogenic influences of the cities, evaluated the quality of raw and treated effluent and the sludge generated in sewage treatment plants, especially with regard to heavy metals. Measurements of metals were performed by Synchrotron Radiation Total Reflection X-ray Fluorescence. For treated effluent data were compared to CONAMA 357 law and Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb showed concentrations in according with the law. To reuse in agriculture the contents were compared to the limits defined by CETESB and some elements had concentrations above to the permitted preventing its reuse. For sludge, Cr, Ni, Cu, Zn, Ba and Pb, in the two treatment plants studied, the concentrations were lower than the maximum permissible values established by CONAMA 375 law allowing the sludge application sludge on agricultural land. (author)

  10. Mineral elements and essential trace elements in blood of seals of the North Sea measured by total-reflection X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Griesel, S.; Mundry, R.; Kakuschke, A.; Fonfara, S.; Siebert, U.; Prange, A.

    2006-01-01

    Mineral and essential trace elements are involved in numerous physiological processes in mammals. Often, diseases are associated with an imbalance of the electrolyte homeostasis. In this study, the concentrations of mineral elements (P, S, K, Ca) and essential trace elements (Fe, Cu, Zn, Se, Rb, Sr) in whole blood of harbor seals (Phoca vitulina) were determined using total-reflection X-ray fluorescence spectrometry (TXRF). Samples from 81 free-ranging harbor seals from the North Sea and two captive seals were collected during 2003-2005. Reference ranges and element correlations for health status determination were derived for P, S, K, Ca, Fe, Cu, and Zn level in whole blood. Grouping the seals by age, gender and sample location the concentration levels of the elements were compared. The blood from two captive seals with signs of diseases and four free-ranging seals showed reduced element levels of P, S, and Ca and differences in element correlation of electrolytes were ascertained. Thus, simultaneous measurements of several elements in only 500 μL volumes of whole blood provide the possibility to obtain information on both, the electrolyte balance and the hydration status of the seals. The method could therefore serve as an additional biomonitoring tool for the health assessment

  11. Analysis in crab tissues and in sediment of estuary from Iguape (Sao Paulo, Brazil) by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Salvador, Marcos J.; Sawazaki, David T.A.; Zucchi, Orgheda L.A. Domingues; Vives, Ana Elisa S. de; Hattori, Gustavo Y.

    2007-01-01

    We report the use of Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF) as a technique for macro, micro and trace elements determination in the tissues of the crab Ulcides cordatus and in the sediments from the Iguape estuary (Sao Paulo, Brazil) for environmental pollution control and toxicological evaluation. The analyses were performed on the U. cordatus (muscles and hepatopancreas) and on sediments from 24 sites of the Iguape estuary (Sao Paulo, Brazil). Tissues and sediments samples were analyzed by SRTXRF after digestion in an open system, using Ga as internal standard. Potassium (K), Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Sr, and Ba were the elements detected in crab hepatopancreas at concentration ranging from 0.516 (Mn) to 2061 (K) mug/g. Muscles samples presented the elements K, Ca, Ti, V, Cr, Fe, Ni, Cu, Zn, Br and Sr at concentrations ranging from 0.043 (Ni) to 1917 (K) mug/g. Potassium (K), Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr, Sn, Ce, and Pb were the elements detected in the sediment samples with concentration between 3.8 (Cu) and 14628 (Fe)mug/g. (author)

  12. Determination of calcium, potassium, manganese, iron, copper and zinc levels in representative samples of two onion cultivars using total reflection X-ray fluorescence and ultrasound extraction procedure

    International Nuclear Information System (INIS)

    Alvarez, J.; Marco, L.M.; Arroyo, J.; Greaves, E.D.; Rivas, R.

    2003-01-01

    The chemical characterization of onion cultivar samples is an important tool for the enhancement of their productivity due to the fact that chemical composition is closed related to the quality of the products. A new sample preparation procedure for elemental characterization is proposed, involving the acid extraction of the analytes from crude samples by means of an ultrasonic bath, avoiding the required digestion of samples in vegetable tissue analysis. The technique of total reflection X-ray fluorescence (TXRF) was successfully applied for the simultaneous determination of the elements Ca, K, Mn, Fe, Cu and Zn. The procedure was compared with the wet ashing and dry ashing procedures for all the elements using multivariate analysis and the Scheffe test. The technique of flame atomic absorption spectrometry (FAAS) was employed for comparison purposes and accuracy evaluation of the proposed analysis method. A good agreement between the two techniques was found when using the dry ashing and ultrasound leaching procedures. The levels of each element found for representative samples of two onion cultivars (Yellow Granex PRR 502 and 438 Granex) were also compared by the same method. Levels of K, Mn and Zn were significantly higher in the 438 Granex cultivar, while levels of Ca, Fe and Cu were significantly higher in the Yellow Granex PRR 502 cultivar

  13. Analysis of some chosen elements of cerebrospinal fluid and serum in amyotrophic lateral sclerosis patients by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Ostachowicz, B.; Lankosz, M.; Tomik, B.; Adamek, D.; Wobrauschek, P.; Streli, C.; Kregsamer, P.

    2006-01-01

    Trace elements play an important role in the human central nervous system. Significant variations of the concentration of trace elements in body fluids may occur in neurodegenerative diseases. In the present work an investigation of the elemental composition of the serum, and the cerebrospinal fluid in amyotrophic lateral sclerosis patients and a control group was performed. For the analysis of the body fluids Total reflection X-ray Fluorescence (TXRF) spectrometry was used. The samples were taken during routine diagnostic procedures. Na, Mg, Cl, K, Ca, Cu, Zn, and Br were determined in both fluids. In order to validate the results of analysis a serum standard reference material was measured. A t-test was applied to check if the mean concentrations of the elements are different for ALS and the control group. For the serum samples higher values for Br were found in the ALS group, for the cerebrospinal fluid lower values of Na, Mg and Zn as well as higher Ca values were found in the ALS group compared to the control group

  14. Analysis of some chosen elements of cerebrospinal fluid and serum in amyotrophic lateral sclerosis patients by total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Ostachowicz, B. [Department of Radiometric Analyses, Faculty of Physic and Applied Computer Science, AGH, University of Science and Technology, Cracow (Poland); Lankosz, M. [Department of Radiometric Analyses, Faculty of Physic and Applied Computer Science, AGH, University of Science and Technology, Cracow (Poland); Tomik, B. [Institute of Neurology, Collegium Medicum, Jagiellonian University, Cracow (Poland); Adamek, D. [Institute of Neurology, Collegium Medicum, Jagiellonian University, Cracow (Poland); Wobrauschek, P. [Atominstitut, Vienna University of Technology, Vienna (Austria); Streli, C. [Atominstitut, Vienna University of Technology, Vienna (Austria)]. E-mail: streli@ati.ac.at; Kregsamer, P. [Atominstitut, Vienna University of Technology, Vienna (Austria)

    2006-11-15

    Trace elements play an important role in the human central nervous system. Significant variations of the concentration of trace elements in body fluids may occur in neurodegenerative diseases. In the present work an investigation of the elemental composition of the serum, and the cerebrospinal fluid in amyotrophic lateral sclerosis patients and a control group was performed. For the analysis of the body fluids Total reflection X-ray Fluorescence (TXRF) spectrometry was used. The samples were taken during routine diagnostic procedures. Na, Mg, Cl, K, Ca, Cu, Zn, and Br were determined in both fluids. In order to validate the results of analysis a serum standard reference material was measured. A t-test was applied to check if the mean concentrations of the elements are different for ALS and the control group. For the serum samples higher values for Br were found in the ALS group, for the cerebrospinal fluid lower values of Na, Mg and Zn as well as higher Ca values were found in the ALS group compared to the control group.

  15. Characterization by Total Reflection X-ray Fluorescence Spectrometry of filtered water into the cave under the Sun Pyramid in Teotihuacan City

    International Nuclear Information System (INIS)

    Martinez, T.; Zarazua, G.; Avila-Perez, P.; Juarez, F.; Cabrera, L.; Martinez, G.

    2008-01-01

    Teotihuacan (50 km north-east Mexico City) was the most important ancient city in Mesoamerica and it flourished 200-750 AC. It is situated in the central part of the Valley of Teotihuacan, in Central Mexico. This study was carried out in the 102 m-long cave under the largest single construction, the massive Sun Pyramid, being located on the east side of the 'Avenue of the Dead', in the northern half-part of the city. The study shows the results of Total Reflection X-ray Fluorescence Spectrometry analysis and other techniques of a water sample obtained from the inside of the cave. The inside temperature ranged between 19 and 22 deg. C; relative humidity was between 98 and 99.3%; water-dropping velocity (water de-sorption capability) was 13.5 μL min -1 . Water samples from wells around the site were analyzed too. Metal concentration in all of the water samples matches the characteristics of the sampling site, well's depth, soil and minerals

  16. Analysis of heavy metals and minerals elements in the turmeric using Total-Reflection X-ray Fluorescence analysis technique and Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    Andriamisetra, V.M.Z.

    2014-01-01

    Currently, many studies demonstrate anti-cancer and anti-inflammatory benefits of turmeric. The aims of this work is to perform analysis of metals such as calcium, chromium, manganese, iron, cobalt, nickel, copper, zinc, arsenic, bromine, rubidium, strontium, cadmium and lead in the turmeric collected from various places in Madagascar. The analysis by total reflection X-ray fluorescence technique is used to determine the concentrations of heavy metals, while the atomic absorption spectrometry is used for the determination of trace elements. Analysis results show that the concentration of calcium in the turmeric is very high, its average concentration is 1025.8 mg.kg -1 . The average concentrations of manganese, of copper and of iron are respectively 44.7 mg.kg -1 ; 19.7 mg.kg -1 and 53.6 mg.kg -1 . The average concentrations of zinc, of rubidium and of strontium are respectively 17.3 mg.kg -1 ; 35.2 mg.kg -1 and 21.7 mg.kg -1 [fr

  17. Characterization by Total Reflection X-ray Fluorescence Spectrometry of filtered water into the cave under the Sun Pyramid in Teotihuacan City

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, T. [National University of Mexico, Faculty of Chemistry, Building D, CU, O4510, Mexico, D.F. (Mexico)], E-mail: tmc@servidor.unam.mx; Zarazua, G.; Avila-Perez, P. [National Institute of Nuclear Research, Carr. Mexico-Toluca Km 36.5, 52045, Salazar, Ocoyoacac, Edo. de Mexico (Mexico); Juarez, F. [National University of Mexico, Institute of Geophysics, Circuito Institutos, CU, 04510 Mexico, D.F. (Mexico); Cabrera, L. [National University of Mexico, Faculty of Chemistry, Building D, CU, O4510, Mexico, D.F. (Mexico); Martinez, G. [Coordinacion Nacional de Conservacion del Patrimonio Cultural, Xicotencatl y General Anaya s/n., 04120, Mexico, D.F. (Mexico)

    2008-12-15

    Teotihuacan (50 km north-east Mexico City) was the most important ancient city in Mesoamerica and it flourished 200-750 AC. It is situated in the central part of the Valley of Teotihuacan, in Central Mexico. This study was carried out in the 102 m-long cave under the largest single construction, the massive Sun Pyramid, being located on the east side of the 'Avenue of the Dead', in the northern half-part of the city. The study shows the results of Total Reflection X-ray Fluorescence Spectrometry analysis and other techniques of a water sample obtained from the inside of the cave. The inside temperature ranged between 19 and 22 deg. C; relative humidity was between 98 and 99.3%; water-dropping velocity (water de-sorption capability) was 13.5 {mu}L min{sup -1}. Water samples from wells around the site were analyzed too. Metal concentration in all of the water samples matches the characteristics of the sampling site, well's depth, soil and minerals.

  18. Quantification of potentially toxic elements in sewage and sludge from treatment plants in the cities of Campinas and Jaguariuna using synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Souza, Luciana Carla Ferreira de; Canteras, Felippe Benavente; Moreira, Silvana

    2013-01-01

    The rapid urban and industrial development in last decades has brought as one of the consequences, changes in the environment. The lack of planning of city growth is, today, one of the major causes of water pollution including residential, industrial, agricultural, and hospital waste. The metals contamination is a major problem, causing serious changes to the environment, causing harm to human health. The sludge generated at sewage treatment plants, is an important source of nutrients and organic matter, and therefore it can also be reused mainly for agricultural use, since contaminants are removed. The cities of Campinas and Jaguariuna are inserted in the Campinas Metropolitan Region (CMR), one of the most dynamic regions in the Brazilian economy. Therefore, to study the anthropogenic influences of the cities, evaluated the quality of raw and treated effluent and the sludge generated in sewage treatment plants, especially with regard to heavy metals. Measurements of metals were performed by Synchrotron Radiation Total Reflection X-ray Fluorescence. For treated effluent data were compared to CONAMA 357 law and Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb showed concentrations in according with the law. To reuse in agriculture the contents were compared to the limits defined by CETESB and some elements had concentrations above to the permitted preventing its reuse. For sludge, Cr, Ni, Cu, Zn, Ba and Pb, in the two treatment plants studied, the concentrations were lower than the maximum permissible values established by CONAMA 375 law allowing the sludge application sludge on agricultural land. (author)

  19. Analysis in crab tissues and in sediment of estuary from Iguape (Sao Paulo, Brazil) by total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Salvador, Marcos J. [Universidade do Vale do Paraiba (UNIVAP), Sao Jose dos Campos, SP (Brazil)], E-mail: mjsalvador1531@yahoo.com.br; Sawazaki, David T.A.; Zucchi, Orgheda L.A. Domingues [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas], E-mail: david_tatsuo@hotmail.com, E-mail: olzucchi@fcfrp.usp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo], E-mail: aesvives@unimep.br; Hattori, Gustavo Y. [Universidade Federal do Amazonas, Benjamin Constant (Brazil). Faculdade de Ciencias Agrarias], E-mail: hattori@ufam.edu.br

    2007-07-01

    We report the use of Synchrotron Radiation Total Reflection X-Ray Fluorescence analysis (SR-TXRF) as a technique for macro, micro and trace elements determination in the tissues of the crab Ulcides cordatus and in the sediments from the Iguape estuary (Sao Paulo, Brazil) for environmental pollution control and toxicological evaluation. The analyses were performed on the U. cordatus (muscles and hepatopancreas) and on sediments from 24 sites of the Iguape estuary (Sao Paulo, Brazil). Tissues and sediments samples were analyzed by SRTXRF after digestion in an open system, using Ga as internal standard. Potassium (K), Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Sr, and Ba were the elements detected in crab hepatopancreas at concentration ranging from 0.516 (Mn) to 2061 (K) mug/g. Muscles samples presented the elements K, Ca, Ti, V, Cr, Fe, Ni, Cu, Zn, Br and Sr at concentrations ranging from 0.043 (Ni) to 1917 (K) mug/g. Potassium (K), Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr, Sn, Ce, and Pb were the elements detected in the sediment samples with concentration between 3.8 (Cu) and 14628 (Fe)mug/g. (author)

  20. Two different preparation techniques for trace element determination of single Daphnia specimen using total reflection x-ray fluorescence analysis (TXRF)

    International Nuclear Information System (INIS)

    Woelfl, S.; Mages, M.

    2000-01-01

    Bio accumulation gives first information about the bio-availability of elements in waters and becomes more and more important for the characterization of the water quality. The use of common analytical techniques like ICP-MS and AAS requires large quantities of biologic sample material. Single preparation for example of Daphnia, a common species for bio-test experiments, are hardly possible with these procedures. Therefore alternatively quantitative TXRF element determination of individually prepared Daphnia was developed. Two preparation techniques for single freshwater crustacean specimen from a eutrophic branch of the river Elbe in the 'Rothehorn Park', Magdeburg (Daphnia: dry weight: 10 - 50 μg individuum -1 ) had been tested: (1) Wet preparation: the single Daphnia specimen had been washed with 0.45 μm filtered lake water and put onto quartz sample carriers. After air drying, the body length were determined in order to calculate the dry weight according to previously established body lengths-dry weight relationships. (2) Dry preparation: after collection specimen were washed with 0.45 μm filtered lake water and frozen in liquid nitrogen. The individual lyophilisated dried Daphnia were weighted using an ultrafine micro-balance and put onto quartz sample carriers. After preparation, addition of some μl Gallium standard solution and air drying the individual Daphnia were digested at the quartz sample carriers with 10 μl HNO 3 on a hot plate and dried once more. Finally the element concentrations were determined using a EXTRA IIA total-reflection x-ray fluorescence spectrometer. As a result of these investigations we can conclude that both, the 'dry' and 'wet' preparation method can be used for the element determination in small single crustaceans using TXRF spectrometry. It seems that the 'dry' method yields more precise results, but the wet method is easier to handle in field when samples cannot be fixed with liquid nitrogen. (author)

  1. Enamel Mineral Content Changes After Bleaching With High and Low Hydrogen Peroxide Concentrations: Colorimetric Spectrophotometry and Total Reflection X-ray Fluorescence Analyses.

    Science.gov (United States)

    Pinto, Avd; Bridi, E C; Amaral, Flb; França, Fmg; Turssi, C P; Pérez, C A; Martinez, E F; Flório, F M; Basting, R T

    The purpose of this study was to evaluate the calcium (Ca) and phosphorous (P) content in enamel bleached with high and low concentrations of hydrogen peroxide (HP) using Total Reflection X-Ray Fluorescence (TXRF) and colorimetric spectrophotometry (SPEC). Forty-eight sound human third molars were used. Their roots were embedded in polystyrene resin and immersed for seven days in an artificial saliva solution. Then they were distributed into six groups to receive the bleaching treatments. The agents of high HP concentration (for in-office use) evaluated were Whiteness HP Maxx/FGM (35% HP), Whiteness HP Blue/FGM (35% HP, 2% calcium gluconate), Pola Office+/SDI (37.5% HP, 5% potassium nitrate), and Opalescence Boost/Ultradent (38% HP, 1.1% ion fluoride, 3% potassium nitrate); these agents were applied to enamel in three sessions. The agents of low HP concentration (for home use) evaluated were Pola Day/SDI (9.5% HP) and White Class 10%/FGM (10% HP, potassium nitrate, calcium, fluoride), and these agents were applied for 14 days. Enamel microbiopsies were evaluated by TXRF and SPEC analysis before the bleaching treatment (baseline), during the treatment, and 14 days after the end of the treatment. For TXRF, the Kruskal-Wallis test showed that Ca and P were not influenced by agent (p>0.05). For SPEC, Pola Office+, Opalescence Boost, Pola Day, and White Class 10% caused a decrease of Ca over time; there was a significant decrease of P over time to Pola Office+ and White Class 10%. The Spearman test showed no correlation between the Ca (p=0.987; r 2 =-0.020) and P (p=0.728, r 2 =0.038) obtained by SPEC and TXRF. For TXRF and SPEC, changes in Ca and P during bleaching occurred independently of the HP concentration used.

  2. Principles of femtosecond X-ray/optical cross-correlation with X-ray induced transient optical reflectivity in solids

    Energy Technology Data Exchange (ETDEWEB)

    Eckert, S., E-mail: sebastian.eckert@helmholtz-berlin.de, E-mail: martin.beye@helmholtz-berlin.de; Beye, M., E-mail: sebastian.eckert@helmholtz-berlin.de, E-mail: martin.beye@helmholtz-berlin.de; Pietzsch, A.; Quevedo, W.; Hantschmann, M. [Institute for Methods and Instrumentation in Synchrotron Radiation Research, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Albert-Einstein-Str. 15, 12489 Berlin (Germany); Ochmann, M.; Huse, N. [Institute for Nanostructure and Solid State Physics, University of Hamburg, Jungiusstr. 11, 20355 Hamburg, Germany and Max Planck Institute for the Structure and Dynamics of Matter, Center for Free-Electron Laser Science, Luruper Chaussee 149, 22761 Hamburg (Germany); Ross, M.; Khalil, M. [Department of Chemistry, University of Washington, Box 351700, Seattle, Washington 98195 (United States); Minitti, M. P.; Turner, J. J.; Moeller, S. P.; Schlotter, W. F.; Dakovski, G. L. [LCLS, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Föhlisch, A. [Institute for Methods and Instrumentation in Synchrotron Radiation Research, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Albert-Einstein-Str. 15, 12489 Berlin (Germany); Institut für Physik und Astronomie, Universität Potsdam, Karl-Liebknecht-Str. 24/25, 14476 Potsdam (Germany)

    2015-02-09

    The discovery of ultrafast X-ray induced optical reflectivity changes enabled the development of X-ray/optical cross correlation techniques at X-ray free electron lasers worldwide. We have now linked through experiment and theory the fundamental excitation and relaxation steps with the transient optical properties in finite solid samples. Therefore, we gain a thorough interpretation and an optimized detection scheme of X-ray induced changes to the refractive index and the X-ray/optical cross correlation response.

  3. Study of air pollution in terms of heavy metals and particulate matter at Ambodin'isotry using the technique of total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    AHMED, H.

    2011-01-01

    The present work is devoted to study the air pollution in terms of particulate matters and heavy metals in Ambodin'isotry in Antananarivo city by the method of total reflection X-ray fluorescence. This work has been done within the Institut National des Sciences et Techniques Nucleaires (Madagascar-INSTN). GENT air sampler has been used for the collections of the aerosol samples. This air sampler is placed at about 7 meters above the ground in order to avoid the contaminations. The samplings were carried out from 14 April to 29 August 2008. The duration of sampling is 24 hours. The results show that the analyzed aerosol samples contain the elements like the titanium , the chromium, the manganese, the iron, the nickel, the copper, the zinc, the bromine, the strontium and the lead. The average concentrations in element lead are lower than the standards ones adopted by the World Health Organization (WHO) (500 ng.m -3 ) and the United States Environmental Protection Agency (US EPA) (1500 ng.m -3 ). The total average concentrations in element lead are lower than the standards ones adopted by the World Health Organization (WHO) (500 ng.m -3 ). The total of average concentrations in lead doesn't present a danger for the population of Ambodin'isotry. The average concentrations of PM10 in the aerosols do not respect the guideline values of 50μg.m -3 adopted by the WHO and the European Union according to the directive 2005 and those of PM 2.5 exceed extensively the guideline values of the WHO (25μg.m -3 ) and of the US EPA (35μg.m -3 ). Consequently, the site of Ambodin'Isotry is polluted in term of airborne particulate matters. The calculation of enrichment factors by Mason's model shows the titanium, the iron, the nickel and the strontium are natural origin while the chromium, the nickel, the copper, the zinc, the bromine and the lead are from anthropogenic sources. [fr

  4. An experimental measurement of metal multilayer x-ray reflectivity degradation due to intense x-ray flux

    International Nuclear Information System (INIS)

    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 0 and 10 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 2 and the integrated energy at destruction was 2.0 J/cm 2 . 82 refs., 66 figs., 10 tabs

  5. X ray reflection masks: Manufacturing, characterization and first tests

    Science.gov (United States)

    Rahn, Stephen

    1992-09-01

    SXPL (Soft X-ray Projection Lithography) multilayer mirrors are characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors with a 2d in the region of 14 nm were characterized by Cu-k(alpha) grazing incidence as well as soft X-ray normal incidence reflectivity measurements. The multilayer mirrors were patterned by reactive ion etching with CF4 using a photoresist as etch mask, thus producing X-ray reflection masks. The masks were tested at the synchrotron radiation laboratory of the electron accelerator ELSA. A double crystal X-ray monochromator was modified so as to allow about 0.5 sq cm of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto a resist and structure sizes down to 8 micrometers were nicely reproduced. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

  6. Calibrating an ellipsometer using x-ray reflectivity

    International Nuclear Information System (INIS)

    Richter, Andrew; Guico, Rodney; Wang, Jin

    2001-01-01

    X-ray reflectivity has been used to find the optical refractive index of polymer thin film in order to calibrate a Stokes ellipsometer for film thickness measurements during the deposition procedure. A thin, spun-cast film of poly(tert-butyl acrylate) (PtBA) was made with a film thickness of ∼500 {angstrom}. An x-ray reflectivity measurement was taken and the data were fit to determine the thickness of the PtBA film and the underlying silicon--oxide layer. This measurement was then used to calculate the optical refractive index for PtBA at the ellipsometer wavelength. Using this value for the refractive index subsequently allowed us to determine the film thickness for a series of PtBA films made by using a number of polymer solution concentrations resulting in film thickness ranging from 100 to 1300 {angstrom}. These film thicknesses were found to be generally the same as those found using x-ray reflectivity. The success of this procedure suggests a useful method for calibrating an ellipsometer for fast in-lab measurements, especially on ultrathin films when simultaneous determination of the film thickness and the refractive index is less reliable

  7. A comparative study on total reflection X-ray fluorescence determination of low atomic number elements in air, helium and vacuum atmospheres using different excitation sources

    Science.gov (United States)

    Misra, N. L.; Kanrar, Buddhadev; Aggarwal, S. K.; Wobrauschek, Peter; Rauwolf, M.; Streli, Christina

    2014-09-01

    A comparison of trace element determinations of low atomic number (Z) elements Na, Mg, Al, P, K and Ca in air, helium and vacuum atmospheres using W Lβ1, Mo Kα and Cr Kα excitations has been made. For Mo Kα and W Lβ1 excitations a Si (Li) detector with beryllium window was used and measurements were performed in air and helium atmospheres. For Cr Kα excitation, a Si (Li) detector with an ultra thin polymer window (UTW) was used and measurements were made in vacuum and air atmospheres. The sensitivities of the elemental X-ray lines were determined using TXRF spectra of standard solutions and processing them by IAEA QXAS program. The elemental concentrations of the elements in other solutions were determined using their TXRF spectra and pre-determined sensitivity values. The study suggests that, using the above experimental set up, Mo Kα excitation is not suited for trace determination of low atomic number element. Excitation by WLβ1 and helium atmosphere, the spectrometer can be used for the determination of elements with Z = 15 (P) and above with fairly good detection limits whereas Cr Kα excitation with ultra thin polymer window and vacuum atmosphere is good for the elements having Z = 11 (Na) and above. The detection limits using this set up vary from 7048 pg for Na to 83 pg for Ti.

  8. Compact X-ray sources: X-rays from self-reflection

    Science.gov (United States)

    Mangles, Stuart P. D.

    2012-05-01

    Laser-based particle acceleration offers a way to reduce the size of hard-X-ray sources. Scientists have now developed a simple scheme that produces a bright flash of hard X-rays by using a single laser pulse both to generate and to scatter an electron beam.

  9. A comparison of the performance of a fundamental parameter method for analysis of total reflection X-ray fluorescence spectra and determination of trace elements, versus an empirical quantification procedure

    Science.gov (United States)

    W(egrzynek, Dariusz; Hołyńska, Barbara; Ostachowicz, Beata

    1998-01-01

    The performance has been compared of two different quantification methods — namely, the commonly used empirical quantification procedure and a fundamental parameter approach — for determination of the mass fractions of elements in particulate-like sample residues on a quartz reflector measured in the total reflection geometry. In the empirical quantification procedure, the spectrometer system needs to be calibrated with the use of samples containing known concentrations of the elements. On the basis of intensities of the X-ray peaks and the known concentration or mass fraction of an internal standard element, by using relative sensitivities of the spectrometer system the concentrations or mass fractions of the elements are calculated. The fundamental parameter approach does not require any calibration of the spectrometer system to be carried out. However, in order to account for an unknown mass per unit area of a sample and sample nonuniformity, an internal standard element is added. The concentrations/mass fractions of the elements to be determined are calculated during fitting a modelled X-ray spectrum to the measured one. The two quantification methods were applied to determine the mass fractions of elements in the cross-sections of a peat core, biological standard reference materials and to determine the concentrations of elements in samples prepared from an aqueous multi-element standard solution.

  10. Reflection of attosecond x-ray free electron laser pulses

    International Nuclear Information System (INIS)

    Hau-Riege, Stefan P.; Chapman, Henry N.

    2007-01-01

    In order to utilize hard x-ray free electron lasers (XFEL's) when they are extended to attosecond pulse lengths, it is necessary to choose optical elements with minimal response time. Specular grazing-incidence optics made of low-Z materials are popular candidates for reflectors since they are likely to withstand x-ray damage and provide sufficiently large reflectivities. Using linear-optics reflection theory, we calculated the transient reflectivity of a delta-function electric pulse from a homogenous semi-infinite medium as a function of angle of incidence for s- and p-polarized light. We specifically considered the pulse response of beryllium, diamond, silicon carbide, and silicon, all of which are of relevance to the XFEL's that are currently being built. We found that the media emit energy in a damped oscillatory way, and that the impulse-response times are shorter than 0.3 fs for normal incidence. For grazing incidence, the impulse-response time is substantially shorter, making grazing-incidence mirrors a good choice for deep subfemtosecond reflective optics

  11. X-ray microscopy using grazing-incidence reflections optics

    International Nuclear Information System (INIS)

    Price, R.H.

    1983-01-01

    The role of Kirkpatrick-Baez microscopes as the workhorse of the x-ray imaging devices is discussed. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics

  12. X-ray microscopy using grazing-incidence reflection optics

    International Nuclear Information System (INIS)

    Price, R.H.

    1981-01-01

    The Kirkpatrick-Baez microscopes are described along with their role as the workhorse of the x-ray imaging devices. This role is being extended with the development of a 22X magnification Kirkpatrick-Baez x-ray microscope with multilayer x-ray mirrors. These mirrors can operate at large angles, high x-ray energies, and have a narrow, well defined x-ray energy bandpass. This will make them useful for numerous experiments. However, where a large solid angle is needed, the Woelter microscope will still be necessary and the technology needed to build them will be useful for many other types of x-ray optics

  13. A laboratory based x-ray reflectivity system

    International Nuclear Information System (INIS)

    Holt, S.A.; Creagh, D.C.; Jamie, I.M.; Dowling, T.L.; Brown, A.S.

    1996-01-01

    Full text: X-ray Reflectivity (XRR) over the last decade has proved to be a versatile and powerful technique by which the thickness of thin films, surface roughness and interface roughness can be determined. The systems amenable to study range from organic monolayers (liquid or solid substrates) to layered metal or semiconductor systems. Access to XRR has been limited by the requirement for synchrotron radiation sources. The development of XRR systems for the laboratory environment was pioneered by Weiss. An X-ray Reflectometer has been constructed by the Department of Physics (Australian Defence Force Academy) and the Research School of Chemistry (Australian National University). The general principles of the design were similar to those described by Weiss. The reflectometer is currently in the early stages of commissioning, with encouraging results thus far. The diffraction pattern of Mobil Catalytic Material (MCM), consisting primarily of SiO 2 . The poster will describe the reflectometer, its operation and present a summary of the most important results obtained to date

  14. Top layer's thickness dependence on total electron-yield X-ray standing-wave

    International Nuclear Information System (INIS)

    Ejima, Takeo; Yamazaki, Atsushi; Banse, Takanori; Hatano, Tadashi

    2005-01-01

    A Mo single-layer film with a stepwise thickness distribution was fabricated on the same Mo/Si reflection multilayer film. Total electron-yield X-ray standing-wave (TEY-XSW) spectra of the aperiodic multilayer were measured with reflection spectra. The peak positions of the standing waves in the TEY-XSW spectra changed as the film thickness of the top Mo-layer increased

  15. X-ray specular reflection and fluorescence study of nano-films

    International Nuclear Information System (INIS)

    Zheludeva, S.; Novikova, N.

    2001-01-01

    The techniques that combine the advantages of high-resolution structure sensitive x-ray methods with spectroscopic selectivity of data obtained are shown to be extremely promising for characterization of organic and inorganic nano films and nano structures. Fluorescence yield angular dependences exited by complicated evanescent wave / x-ray standing wave pattern at total reflection and glancing incidence can be used to detect structure position of different ions in organic systems and alien interfacial layers in inorganic multilayers;, to get information about interdiffusion at the interfaces of Langmuir- Blodgett (L-B) films and artificial inorganic - x-ray mirrors; to study ion permeation through L-B nano structures - models of biomembrans; to obtain nano - film thickness and density; to get precisely the parameters of small d-space multilayer mirrors, ets

  16. Evaluation of water and sediment of the Graminha and Aguas da Serra streams in the city of Limeira (Sp-Brazil) by Synchrotron Radiation Total Reflection X-ray Fluorescence

    International Nuclear Information System (INIS)

    Moreira, Silvana; Fazza, Elizete Vieira

    2008-01-01

    The city of Limeira is located in the state of Sao Paulo, Brazil and has the second largest economy and demographic growth of the state. It comprises an expressive economy with industries in several productive sectors. The source of the Graminha and Aguas da Serra streams is located within the Limeira urban zone. The streams cross part of the rural zone and unite by draining into the Piracicaba River. It is possible that these basins suffer or have already suffered the impacts of environmental pollution caused by anthropogenic factors. Since the city has galvanization industries for the production of precious and semi-precious jewels as well as imitation jewelry, the concentration descriptions and interpretations of heavy metals in waters and sediments indicate anthropogenic influence and the dumping of these compounds into the Piracicaba River. The Synchrotron Radiation Total Reflection X-Ray Fluorescence (SR-TXRF) was used for determining the metals. All measurements were performed using a white beam of synchrotron radiation for excitation and a Ge hyperpure detector. Detection limits for water samples were 0.04 μg L -1 and in sediment samples 0.03 μg g -1 for Cu and Zn elements. In the water samples, concentrations higher than permissible as established by the Brazilian legislation (CONAMA) for Al, Fe, Zn, Cr, Ni, Cu and Pb, were observed. For sediment samples, values higher than quality reference values defined by the Brazilian legislation (CETESB) were verified for Cr, Zn, Cu, Ni and Pb

  17. Evaluation of water and sediment of the Graminha and Aguas da Serra streams in the city of Limeira (Sp-Brazil) by Synchrotron Radiation Total Reflection X-ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana [University of Campinas, School of Civil Engineering, Architecture and Urban Design, P. O. Box 602, Zip Code 13083-852, Campinas, SP (Brazil)], E-mail: silvana@fec.unicamp.br; Fazza, Elizete Vieira [University of Campinas, School of Civil Engineering, Architecture and Urban Design, P. O. Box 602, Zip Code 13083-852, Campinas, SP (Brazil)], E-mail: fazzaelizete@yahoo.com

    2008-12-15

    The city of Limeira is located in the state of Sao Paulo, Brazil and has the second largest economy and demographic growth of the state. It comprises an expressive economy with industries in several productive sectors. The source of the Graminha and Aguas da Serra streams is located within the Limeira urban zone. The streams cross part of the rural zone and unite by draining into the Piracicaba River. It is possible that these basins suffer or have already suffered the impacts of environmental pollution caused by anthropogenic factors. Since the city has galvanization industries for the production of precious and semi-precious jewels as well as imitation jewelry, the concentration descriptions and interpretations of heavy metals in waters and sediments indicate anthropogenic influence and the dumping of these compounds into the Piracicaba River. The Synchrotron Radiation Total Reflection X-Ray Fluorescence (SR-TXRF) was used for determining the metals. All measurements were performed using a white beam of synchrotron radiation for excitation and a Ge hyperpure detector. Detection limits for water samples were 0.04 {mu}g L{sup -1} and in sediment samples 0.03 {mu}g g{sup -1} for Cu and Zn elements. In the water samples, concentrations higher than permissible as established by the Brazilian legislation (CONAMA) for Al, Fe, Zn, Cr, Ni, Cu and Pb, were observed. For sediment samples, values higher than quality reference values defined by the Brazilian legislation (CETESB) were verified for Cr, Zn, Cu, Ni and Pb.

  18. Analysis of trace and mineral elements in vanilla pods from the region of S.A.V.A using total reflection X-ray fluorescence, atomic absorption and ion chromatography techniques

    International Nuclear Information System (INIS)

    Be, K.

    2013-01-01

    In the case of studies of food security, - arsenic, cobalt, chromium, copper, iron, manganese, nickel, rubidium, selenium, strontium, titanium, zinc - cadmium, lead - are almost always analyzed. Guide values are used to express the level of quality in matter of consumption. Analytical laboratories of Madagascar-INSTN outline usually their research on quantifying those elements by using two different analytical methods, the Total Reflection X-Ray Fluorescence for the first twelve metals and the Atomic Absorption Spectrometry dedicated to lead and cadmium. Supplementary analysis is carried out for the quantification of essential mineral elements such as calcium, magnesium and potassium by using Ion Chromatograph. The aim of this study was to set up the analysis of the above mentioned elements in vanilla pods collected from Sambava, Antalaha and Andapa for a routine use. After all the parameters were established, the validation was particularly focused on the limits of detection and quantification and the accuracy of each element. The used methods fulfil the scope of application needed and are easy to use in routine. [fr

  19. A new technique for the deposition of standard solutions in total reflection X-ray fluorescence spectrometry (TXRF) using pico-droplets generated by inkjet printers and its applicability for aerosol analysis with SR-TXRF

    International Nuclear Information System (INIS)

    Fittschen, U.E.A.; Hauschild, S.; Amberger, M.A.; Lammel, G.; Streli, C.; Foerster, S.; Wobrauschek, P.; Jokubonis, C.; Pepponi, G.; Falkenberg, G.; Broekaert, J.A.C.

    2006-01-01

    A new technique for the deposition of standard solutions on particulate aerosol samples using pico-droplets for elemental determinations with total reflection X-ray fluorescence spectrometry (TXRF) is described. It enables short analysis times without influencing the sample structure and avoids time consuming scanning of the sample with the exciting beam in SR-TXRF analysis. Droplets of picoliter volume (∼ 5-130 pL) were generated with commercially available and slightly modified inkjet printers operated with popular image processing software. The size of the dried droplets on surfaces of different polarity namely silicone coated and untreated quartz reflectors, was determined for five different printer types and ten different cartridge types. The results show that droplets generated by inkjet printers are between 50 and 200 μm in diameter (corresponding to volumes of 5 to 130 pL) depending on the cartridge type, which is smaller than the width of the synchrotron beam used in the experiments (< 1 mm at an energy of 17 keV at the beamline L at HASYLAB, Hamburg). The precision of the printing of a certain amount of a single element standard solution was found to be comparable to aliquoting with micropipettes in TXRF, where for 2.5 ng of cobalt relative standard deviations of 12% are found. However, it could be shown that the printing of simple patterns is possible, which is important when structured samples have to be analysed

  20. Ionic liquids: an x-ray reflectivity study

    International Nuclear Information System (INIS)

    Sloutskin, E.; Deutsch, M.; Tamam, L.; Ocko, B.; Kuzmenko, I.; Gog, T.

    2005-01-01

    Full Text:Ionic liquids are non-volatile, non-flammable and thermally stable solvents, and as such are promising 'green' replacements for traditional volatile organic solvents. In the last years hundreds of Ionic liquids were synthesized. Due to the Ionic liquids great industrial potential, this number is growing at an exceedingly fast rate. Despite the great importance of the interfacial properties of materials for technological applications and basic science, the atomic-scale surface structure of the Ionic liquids has never been studied previously. In our study, synchrotron x-ray reflectivity and surface tensiometry were employed to obtain the surface structure and thermodynamics of two ionic liquids, based on the 1-alkyl-3-methylimidazolium cations. A molecular layer of a density ∼18% higher than that of the bulk is found to form at the free surface of these liquids. The excess concentration of the oppositely charged ions within the surface layer is determined by chemical substitution of the anion. Finally, the observed layering at the surface is contrasted with our measurements on the behavior of classical aqueous salt solutions

  1. The influence of the solid waste disposal areas in Campinas city, Sao Paulo state (Brazil) on water quality: determination of metals using synchrotron radiation total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Oliveira, Bruna F.F.; Moreira, Silvana; Canteras, Felippe Benavente

    2013-01-01

    Among the many forms of waste disposal, landfills today are best suited to Brazilian conditions, this because their construction allows minimizing the negative effects of landfill gas and slurry produced. However, the confinement of pollutants from landfills is linked to its construction and operation and when the construction and/or is wrong they can endanger air, groundwater and surface waters qualities. Thus, the main objective of this study was to analyze the concentration of heavy metals in samples of groundwater, surface water and slurry coming from solid waste disposal locations in the city of Campinas, SP - Delta, Santa Barbara and Pirelli Landfills. The samples were analyzed at the Brazilian Synchrotron Light Laboratory using Synchrotron Radiation Total Reflection X-Ray Fluorescence technique (SR-TXRF). In Pirelli Landfill, the highest concentrations were observed in one of the wells located to downstream of the Landfill (in relation to the groundwater flux) - the monitoring well PM04, exceeding the intervention value defined by CETESB. For Santa Barbara landfill in one upstream monitoring well the concentrations of Ni, Mn, Pb and Cr, surpassed the maximum permissive values. The manganese in Landfill Delta showed to be higher in wells located downstream and 50% of the wells analyzed exceeded the maximum permissive value for groundwater samples. In the case of surface waters located in the vicinity of landfill sites, the metals that surpassed the maximum permissive values according the legislation in most of the points analyzed were Mn, Cu and Pb. For slurry samples collected in Delta Landfill, the average concentrations for Mn, Ni, Cu and Pb not exceeded the maximum permissive values during the period studied. Moreover for Santa Barbara the average concentration of Mn, Cu and Zn surpassed the permissive limits, as was observed for Mn in the Pirelli Landfill. (author)

  2. Single-particle characterization of summertime Antarctic aerosols collected at King George Island using quantitative energy-dispersive electron probe X-ray microanalysis and attenuated total reflection Fourier transform-infrared imaging techniques.

    Science.gov (United States)

    Maskey, Shila; Geng, Hong; Song, Young-Chul; Hwang, Heejin; Yoon, Young-Jun; Ahn, Kang-Ho; Ro, Chul-Un

    2011-08-01

    Single-particle characterization of Antarctic aerosols was performed to investigate the impact of marine biogenic sulfur species on the chemical compositions of sea-salt aerosols in the polar atmosphere. Quantitative energy-dispersive electron probe X-ray microanalysis was used to characterize 2900 individual particles in 10 sets of aerosol samples collected between March 12 and 16, 2009 at King Sejong Station, a Korean scientific research station located at King George Island in the Antarctic. Two size modes of particles, i.e., PM(2.5-10) and PM(1.0-2.5), were analyzed, and four types of particles were identified, with sulfur-containing sea-salt particles being the most abundant, followed by genuine sea-salt particles without sulfur species, iron-containing particles, and other species including CaCO(3)/CaMg(CO(3))(2), organic carbon, and aluminosilicates. When a sulfur-containing sea-salt particle showed an atomic concentration ratio of sulfur to sodium of >0.083 (seawater ratio), it is regarded as containing nonsea-salt sulfate (nss-SO(4)(2-)) and/or methanesulfonate (CH(3)SO(3)(-)), which was supported by attenuated total reflection Fourier transform-infrared imaging measurements. These internal mixture particles of sea-salt/CH(3)SO(3)(-)/SO(4)(2-) were very frequently encountered. As nitrate-containing particles were not encountered, and the air-masses for all of the samples originated from the Pacific Ocean (based on 5-day backward trajectories), the oxidation of dimethylsulfide (DMS) emitted from phytoplanktons in the ocean is most likely to be responsible for the formation of the mixed sea-salt/CH(3)SO(3)(-)/SO(4)(2-) particles.

  3. Two-axis Neutron and X-ray Reflectivity

    DEFF Research Database (Denmark)

    Bouwman, W.G.; Vigild, M.E.; Findeisen, E.

    1997-01-01

    Sample alignment for neutron (and in some cases x-ray) reflectometry can be complicated due to a coupling between angle and position which occurs when slits are used to define the path of the beam. Misalignments in sample position or sample rotation angle give rise to systematic errors in the exp...

  4. Controllable reflection of X-rays on crystals of saccharose

    CERN Document Server

    Navasardyan, M A; Hayrapetyan, K T; Gabrielyan, R T

    2003-01-01

    Multiple (ten times and more) increase in intensities of separate reflections and of lauegram reflections from organic single crystals of saccharose (C sub 1 2H sub 2 2O sub 1 1) was observed under influence of certain temperature gradient. On the base of the present experiment and the data of our previous woks we show that the controllable reflection process has a common nature and the intensity of the diffracted beam under external influences does not depend on the total number of electrons per unit volume of the unit cell of the single crystal.

  5. Reflectivity and diffraction of X rays applied to organic thin films

    International Nuclear Information System (INIS)

    Rieutord, Francois

    1987-01-01

    This research thesis reports the study of organic thin films by using X-ray-based technologies, and more particularly X-ray reflectivity. After some recalls on X ray diffraction, and on the fabrication of Langmuir-Blodgett films, the author shows how, by combining three X-ray-based techniques, it is possible to study a volume structure of a thin film. He describes the technique of measurement by X- ray reflexivity, its experimental implementation, and methods for result interpretation. In the next part, the author reports the study of peculiar interference effects which are noticed in reflexivity on Langmuir-Blodgett films, and then describes the nature of these films by correlating results of X ray reflexivity with direct observations performed by electronic microscopy on replica [fr

  6. Interaction between lipid monolayers and poloxamer 188: An X-ray reflectivity and diffraction study

    DEFF Research Database (Denmark)

    Wu, G.H.; Majewski, J.; Ege, C.

    2005-01-01

    The mechanism by which poloxamer 188 (P188) seals a damaged cell membrane is examined using the lipid monolayer as a model system. X-ray reflectivity and grazing-incidence x-ray diffraction results show that at low nominal lipid density, P188, by physically occupying the available area and phase ...

  7. Combined evaluation of grazing incidence X-ray fluorescence and X-ray reflectivity data for improved profiling of ultra-shallow depth distributions

    Energy Technology Data Exchange (ETDEWEB)

    Ingerle, D., E-mail: dingerle@ati.ac.at [Atominstitut, Vienna University of Technology, Stadionallee 2, A-1020 Vienna (Austria); Meirer, F. [Inorganic Chemistry and Catalysis, Debye Institute for Nanomaterials Science, Utrecht University, Universiteitsweg 99, 3584 CG Utrecht (Netherlands); Pepponi, G.; Demenev, E.; Giubertoni, D. [MiNALab, CMM-irst, Fondazione Bruno Kessler, Via Sommarive 18, I-38050 Povo (Italy); Wobrauschek, P.; Streli, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, A-1020 Vienna (Austria)

    2014-09-01

    The continuous downscaling of the process size for semiconductor devices pushes the junction depths and consequentially the implantation depths to the top few nanometers of the Si substrate. This motivates the need for sensitive methods capable of analyzing dopant distribution, total dose and possible impurities. X-ray techniques utilizing the external reflection of X-rays are very surface sensitive, hence providing a non-destructive tool for process analysis and control. X-ray reflectometry (XRR) is an established technique for the characterization of single- and multi-layered thin film structures with layer thicknesses in the nanometer range. XRR spectra are acquired by varying the incident angle in the grazing incidence regime while measuring the specular reflected X-ray beam. The shape of the resulting angle-dependent curve is correlated to changes of the electron density in the sample, but does not provide direct information on the presence or distribution of chemical elements in the sample. Grazing Incidence XRF (GIXRF) measures the X-ray fluorescence induced by an X-ray beam incident under grazing angles. The resulting angle dependent intensity curves are correlated to the depth distribution and mass density of the elements in the sample. GIXRF provides information on contaminations, total implanted dose and to some extent on the depth of the dopant distribution, but is ambiguous with regard to the exact distribution function. Both techniques use similar measurement procedures and data evaluation strategies, i.e. optimization of a sample model by fitting measured and calculated angle curves. Moreover, the applied sample models can be derived from the same physical properties, like atomic scattering/form factors and elemental concentrations; a simultaneous analysis is therefore a straightforward approach. This combined analysis in turn reduces the uncertainties of the individual techniques, allowing a determination of dose and depth profile of the implanted

  8. Off-plane x-ray reflection grating fabrication

    Science.gov (United States)

    Peterson, Thomas J.; DeRoo, Casey T.; Marlowe, Hannah; McEntaffer, Randall L.; Miles, Drew M.; Tutt, James H.; Schultz, Ted B.

    2015-09-01

    Off-plane X-ray diffraction gratings with precision groove profiles at the submicron scale will be used in next generation X-ray spectrometers. Such gratings will be used on a current NASA suborbital rocket mission, the Off-plane Grating Rocket Experiment (OGRE), and have application for future grating missions. The fabrication of these gratings does not come without challenges. High performance off-plane gratings must be fabricated with precise radial grating patterns, optically at surfaces, and specific facet angles. Such gratings can be made using a series of common micro-fabrication techniques. The resulting process is highly customizable, making it useful for a variety of different mission architectures. In this paper, we detail the fabrication method used to produce high performance off-plane gratings and report the results of a preliminary qualification test of a grating fabricated in this manner. The grating was tested in the off-plane `Littrow' configuration, for which the grating is most efficient for a given diffraction order, and found to achieve 42% relative efficiency in the blaze order with respect to all diffracted light.

  9. Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

    International Nuclear Information System (INIS)

    Singh, Surendra; Basu, Saibal

    2016-01-01

    X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependent structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.

  10. Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

    Science.gov (United States)

    Singh, Surendra; Basu, Saibal

    2016-05-01

    X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependent structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.

  11. Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Surendra, E-mail: surendra@barc.gov.in; Basu, Saibal [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 India (India)

    2016-05-23

    X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependent structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.

  12. Simultaneous analysis of Grazing Incidence X-Ray reflectivity and X-ray standing waves from periodic multilayer systems

    NARCIS (Netherlands)

    Yakunin, S.N.; Makhotkin, Igor Alexandrovich; Chuyev, M.A.; Seregin, A.Y.; Pashayev, E.M.; Louis, Eric; van de Kruijs, Robbert Wilhelmus Elisabeth; Bijkerk, Frederik; Kovalchuk, M.V.

    2012-01-01

    Structural analysis of periodic multilayers with small period thickness (~4 nm) is a challenging task, especially when thicknesses of intermixed interfaces become comparable to individual layer thicknesses. In general, angular dependent X-ray fluorescence measurements, excited by the X-ray standing

  13. Determination of Cr, Mn, Fe, Co, Ni, Cu, Zn and As in the Rimac River waters by x-ray fluorescence in total reflection; Determinacion de Cr, Mn, Fe, Co, Ni, Cu, Zn y As en aguas del Rio Rimac por fluorescencia de rayos-x en reflexion total

    Energy Technology Data Exchange (ETDEWEB)

    Tiznado, W [Universidad Nacional Federico Villarreal, Lima (Peru). Facultad de Ciencias Naturales y Matematicas, EP Quimica; Olivera, P [Instituto Peruano de Energia Nuclear, Lima (Peru). Departamento de Quimica

    2002-07-01

    Samples from thirteen stations of the Rimac River has been analyzed. Samples were performed during one-year-period (september 1998-august 1999), with a frequency of one sample per month. The X-ray fluorescence analysis in total reflection technique has been used in order to determine the Cr, Mn, Fe, Co, Ni, Cu, Zn and As elements on its dissolved phase. The results obtained show: relation of the presence of mining stations with the metal concentration level, specially in the Zn and Fe; As is present in concentrations above those of permissible maximum levels in some of the sampled stations; moreover, Ni and Cr, toxic elements, are found in very low concentrations. On the other hand, it has been proved that the analysis method used is useful as a monitoring tool of superficial water-quality due to its low detection limits and because of the fastness the analysis are made.

  14. Study of Cr/Sc-based multilayer reflecting mirrors using soft x-ray reflectivity and standing wave-enhanced x-ray fluorescence

    Science.gov (United States)

    Wu, Meiyi; Burcklen, Catherine; André, Jean-Michel; Guen, Karine Le; Giglia, Angelo; Koshmak, Konstantin; Nannarone, Stefano; Bridou, Françoise; Meltchakov, Evgueni; Rossi, Sébastien de; Delmotte, Franck; Jonnard, Philippe

    2017-11-01

    We study Cr/Sc-based multilayer mirrors designed to work in the water window range using hard and soft x-ray reflectivity as well as x-ray fluorescence enhanced by standing waves. Samples differ by the elemental composition of the stack, the thickness of each layer, and the order of deposition. This paper mainly consists of two parts. In the first part, the optical performances of different Cr/Sc-based multilayers are reported, and in the second part, we extend further the characterization of the structural parameters of the multilayers, which can be extracted by comparing the experimental data with simulations. The methodology is detailed in the case of Cr/B4C/Sc sample for which a three-layer model is used. Structural parameters determined by fitting reflectivity curve are then introduced as fixed parameters to plot the x-ray standing wave curve, to compare with the experiment, and confirm the determined structure of the stack.

  15. Optical and x-ray alignment approaches for off-plane reflection gratings

    Science.gov (United States)

    Allured, Ryan; Donovan, Benjamin D.; DeRoo, Casey T.; Marlowe, Hannah R.; McEntaffer, Randall L.; Tutt, James H.; Cheimets, Peter N.; Hertz, Edward; Smith, Randall K.; Burwitz, Vadim; Hartner, Gisela; Menz, Benedikt

    2015-09-01

    Off-plane reflection gratings offer the potential for high-resolution, high-throughput X-ray spectroscopy on future missions. Typically, the gratings are placed in the path of a converging beam from an X-ray telescope. In the off-plane reflection grating case, these gratings must be co-aligned such that their diffracted spectra overlap at the focal plane. Misalignments degrade spectral resolution and effective area. In-situ X-ray alignment of a pair of off-plane reflection gratings in the path of a silicon pore optics module has been performed at the MPE PANTER beamline in Germany. However, in-situ X-ray alignment may not be feasible when assembling all of the gratings required for a satellite mission. In that event, optical methods must be developed to achieve spectral alignment. We have developed an alignment approach utilizing a Shack-Hartmann wavefront sensor and diffraction of an ultraviolet laser. We are fabricating the necessary hardware, and will be taking a prototype grating module to an X-ray beamline for performance testing following assembly and alignment.

  16. In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

    International Nuclear Information System (INIS)

    Bertram, F.; Evertsson, J.; Messing, M. E.; Mikkelsen, A.; Lundgren, E.; Zhang, F.; Pan, J.; Carlà, F.; Nilsson, J.-O.

    2014-01-01

    We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

  17. X-ray reflectivity measurements of liquid/solid interfaces under high hydrostatic pressure conditions.

    Science.gov (United States)

    Wirkert, Florian J; Paulus, Michael; Nase, Julia; Möller, Johannes; Kujawski, Simon; Sternemann, Christian; Tolan, Metin

    2014-01-01

    A high-pressure cell for in situ X-ray reflectivity measurements of liquid/solid interfaces at hydrostatic pressures up to 500 MPa (5 kbar), a pressure regime that is particularly important for the study of protein unfolding, is presented. The original set-up of this hydrostatic high-pressure cell is discussed and its unique properties are demonstrated by the investigation of pressure-induced adsorption of the protein lysozyme onto hydrophobic silicon wafers. The presented results emphasize the enormous potential of X-ray reflectivity studies under high hydrostatic pressure conditions for the in situ investigation of adsorption phenomena in biological systems.

  18. X-Ray Reflectivity from the Surface of a Liquid Crystal:

    DEFF Research Database (Denmark)

    Pershan, P.S.; Als-Nielsen, Jens Aage

    1984-01-01

    X-ray reflectivity from the surface of a nematic liquid crystal is interpreted as the coherent superposition of Fresnel reflection from the surface and Bragg reflection from smectic order induced by the surface. Angular dependence of the Fresnel effect yields information on surface structure....... Measurement of the intensity of diffuse critical scattering relative to the Fresnel reflection yields the absolute value of the critical part of the density-density correlation function....

  19. Uranium soft x-ray total attenuation coefficients

    International Nuclear Information System (INIS)

    Del Grande, N.K.; Oliver, A.J.

    1981-01-01

    Uranium total attenuation coefficients were measured continuously from 0.84 to 6.0 keV and at selected higher energies using a vacuum single crystal diffractometer and flow-proportional counter. Statistical fluctuations ranged from 0.5% to 2%. The overall accuracy was 3%. Prominent structure was measured within 20 eV of the M 5 (3.552 keV) and M 4 (3.728 keV) edges. Jump ratios were determined from log-log polynomial fits to data at energies apart from the near-edge regions. These data were compared with calculations based on a relativistic HFS central potential model and with previously tabulated data

  20. Cr/B{sub 4}C multilayer mirrors: Study of interfaces and X-ray reflectance

    Energy Technology Data Exchange (ETDEWEB)

    Burcklen, C.; Meltchakov, E.; Jérome, A.; Rossi, S. de; Delmotte, F. [Laboratoire Charles Fabry, Institut d' Optique Graduate School, CNRS, Université Paris-Saclay, 91127 Palaiseau Cedex (France); Soufli, R. [Laboratoire Charles Fabry, Institut d' Optique Graduate School, CNRS, Université Paris-Saclay, 91127 Palaiseau Cedex (France); Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94550 (United States); Dennetiere, D.; Polack, F.; Capitanio, B.; Thomasset, M. [Synchrotron SOLEIL, L' Orme des Merisiers, Saint Aubin, BP 48F-91192 Gif sur Yvette Cedex (France); Gullikson, E. [Center for X-ray Optics, Lawrence Berkeley National Laboratory, 1 Cyclotron Rd., Berkeley, California 94720 (United States)

    2016-03-28

    We present an experimental study of the effect of layer interfaces on the x-ray reflectance in Cr/B{sub 4}C multilayer interference coatings with layer thicknesses ranging from 0.7 nm to 5.4 nm. The multilayers were deposited by magnetron sputtering and by ion beam sputtering. Grazing incidence x-ray reflectometry, soft x-ray reflectometry, and transmission electron microscopy reveal asymmetric multilayer structures with a larger B{sub 4}C-on-Cr interface, which we modeled with a 1–1.5 nm thick interfacial layer. Reflectance measurements in the vicinity of the Cr L{sub 2,3} absorption edge demonstrate fine structure that is not predicted by simulations using the currently tabulated refractive index (optical constants) values for Cr.

  1. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction

    International Nuclear Information System (INIS)

    Fernandes, P.

    2007-04-01

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B 2 liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B 2 phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation

  2. The single reflection regime of X-rays travelling into a monocapillary

    International Nuclear Information System (INIS)

    Dabagov, S.B.; Marcelli, A.

    1999-01-01

    In this manuscript an analysis of the transmission of x-rays through a single monocapillary under the single reflection regime is presented and discussed. Because ray tracing does not allow to explain the experimental data, a first qualitative interpretation of the observed behavior is given in the framework of the wave theory

  3. X-Ray Topography of the Subsurface Crystal Layers in the Skew Asymmetric Reflection Geometry

    Directory of Open Access Journals (Sweden)

    Swiątek Z.

    2016-12-01

    Full Text Available The technique of X ray topography with the asymmetric reflection geometry of X-ray diffraction presented in this paper as useful tool for structural characterization of materials, particularly, epitaxial thin films and semiconductor multi-layered crystal systems used for the optoelectronic devices. New possibilities of this technique for a layer-by-layer visualization of structural changes in the subsurface crystal layers are demonstrated for semiconductors after various types of surface treatment, such as chemical etching, laser irradiation and ion implantation.

  4. Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions

    International Nuclear Information System (INIS)

    Roberts, G.A.; Stewart, K.D.

    2004-01-01

    The design and operation of an electrochemical cell for reflection-mode powder x-ray diffraction experiments are discussed. The cell is designed for the study of electrodes that are used in rechargeable lithium batteries. It is designed for assembly in a glove box so that air-sensitive materials, such as lithium foil electrodes and carbonate-based electrolytes with lithium salts, can be used. The cell uses a beryllium window for x-ray transmission and electrical contact. A simple mechanism for compressing the electrodes is included in the design. Sample results for the cell are shown with a Cu Kα source and a position-sensitive detector

  5. Reflection of femtosecond pulses from soft X-ray free-electron laser by periodical multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Ksenzov, D.; Grigorian, S.; Pietsch, U. [Faculty of Physics, University of Siegen (Germany); Hendel, S.; Bienert, F.; Sacher, M.D.; Heinzmann, U. [Faculty of Physics, University of Bielefeld (Germany)

    2009-08-15

    Recent experiments on a soft X-ray free-electron laser (FEL) source (FLASH in Hamburg) have shown that multilayers (MLs) can be used as optical elements for highly intense X-ray irradiation. An effort to find most appropriate MLs has to consider the femtosecond time structure and the particular photon energy of the FEL. In this paper we have analysed the time response of 'low absorbing' MLs (e.g. such as La/B{sub 4}C) as a function of the number of periods. Interaction of a pulse train of Gaussian shaped sub-pulses using a realistic ML grown by electron-beam evaporation technique has been analysed in the soft-X-ray range. The structural parameters of the MLs were obtained by reflectivity measurements at BESSY II and subsequent profile fittings. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  6. Measured reflectance of graded multilayer mirrors designed for astronomical hard X-ray telescopes

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Craig, W.W.; Windt, D.L.

    2000-01-01

    Future astronomical X-ray telescopes, including the balloon-borne High-Energy Focusing Telescope (HEFT) and the Constellation-X Hard X-ray Telescope (Con-X HXT) plan to incorporate depth-graded multilayer coatings in order to extend sensitivity into the hard X-ray (10 less than or similar to E less......-graded W/Si multilayers optimized for broadband performance up to 69.5 keV (WK-edge). These designs are ideal for both the HEFT and Con-X HXT applications. We compare the measurements to model calculations to demonstrate that the reflectivity can be well described by the intended power law distribution...

  7. On the X-ray reflectivity by poly allyl diglycol carbonate (PADC)

    International Nuclear Information System (INIS)

    Ghazaly, M. El

    2011-01-01

    X-ray reflectivity via the poly allyl diglycol carbonate (CR-39 polymer sheet) was investigated. X-ray reflectivity was measured for a pristine and a chemically etched CR-39 detector in 6.25N NaOH at (70 ± 0.5) .deg. C for different durations. Far from the spectral peak, the reflectivity of the CR-39 polymer sheet has a wide peak at 2θ = 20.1 .deg. , and its intensity is decreased by increasing the etching time. Moreover, the integrated counts under the peaks, C(t e ), vary linearly as a function of the etching time t e . Data are fitted using a linear function C(t e ) = A+Bt e , with fitting parameters A = (3271 ± 170) and B = (- 960 ± 84). The reflectivity deterioration is attributed to the increase of CR-39 surface's roughness due to the chemical etching. The rocking curves of X-ray reflectivity were measured for a pristine and an etched CR-39 polymer sheet. Specular reflections are observed, as well as Yoneda wings, which broaden and move away from the specular reflections due to the increase in the CR-39 surface's roughness.

  8. X-ray Reflected Spectra from Accretion Disk Models. III. A Complete Grid of Ionized Reflection Calculations

    Science.gov (United States)

    Garcia, J.; Dauser, T.; Reynolds, C. S.; Kallman, T. R.; McClintock, J. E.; Wilms, J.; Ekmann, W.

    2013-01-01

    We present a new and complete library of synthetic spectra for modeling the component of emission that is reflected from an illuminated accretion disk. The spectra were computed using an updated version of our code xillver that incorporates new routines and a richer atomic data base. We offer in the form of a table model an extensive grid of reflection models that cover a wide range of parameters. Each individual model is characterized by the photon index Gamma of the illuminating radiation, the ionization parameter zeta at the surface of the disk (i.e., the ratio of the X-ray flux to the gas density), and the iron abundance A(sub Fe) relative to the solar value. The ranges of the parameters covered are: 1.2 <= Gamma <= 3.4, 1 <= zeta <= 104, and 0.5 <= A(sub Fe) <= 10. These ranges capture the physical conditions typically inferred from observations of active galactic nuclei, and also stellar-mass black holes in the hard state. This library is intended for use when the thermal disk flux is faint compared to the incident power-law flux. The models are expected to provide an accurate description of the Fe K emission line, which is the crucial spectral feature used to measure black hole spin. A total of 720 reflection spectra are provided in a single FITS file suitable for the analysis of X-ray observations via the atable model in xspec. Detailed comparisons with previous reflection models illustrate the improvements incorporated in this version of xillver.

  9. X-ray reflectivity study of thermal capillary waves on liquid surfaces

    International Nuclear Information System (INIS)

    Ocko, B.M.; Wu, X.Z.; Sirota, E.B.; Sinha, S.K.; Deutsch, M.

    1994-01-01

    X-ray reflectivity measurements have been carried out at the liquid/vapor interface of normal alkanes. The reflectivities over a large temperature range of different chain lengths (C20 and C36) provide a critical test of the various capillary wave models. Our data are most consistent with the hybrid model which allows for a molecular size dependent cutoff q max for the capillary waves and an intrinsic interface width σ 0

  10. The influence of x-ray energy on lung dose uniformity in total-body irradiation

    International Nuclear Information System (INIS)

    Ekstrand, Kenneth; Greven, Kathryn; Wu Qingrong

    1997-01-01

    Purpose: In this study we examine the influence of x-ray energy on the uniformity of the dose within the lung in total-body irradiation treatments in which partial transmission blocks are used to control the lung dose. Methods and Materials: A solid water phantom with a cork insert to simulate a lung was irradiated by x-rays with energies of either 6, 10, or 18 MV. The source to phantom distance was 3.9 meters. The cork insert was either 10 cm wide or 6 cm wide. Partial transmission blocks with transmission factors of 50% were placed anterior to the cork insert. The blocks were either 8 or 4 cm in width. Kodak XV-2 film was placed in the midline of the phantom to record the dose. Midplane dose profiles were measured with a densitometer. Results: For the 10 cm wide cork insert the uniformity of the dose over 80% of the block width varied from 6.6% for the 6 MV x-rays to 12.2% for the 18 MV x-rays. For the 6 cm wide cork insert the uniformity was comparable for all three x-ray energies, but for 18 MV the central dose increased by 9.4% compared to the 10 cm wide insert. Conclusion: Many factors must be considered in optimizing the dose for total-body irradiation. This study suggests that for AP/PA techniques lung dose uniformity is superior with 6 MV irradiation. The blanket recommendation that the highest x-ray energy be used in TBI is not valid for all situations

  11. The X-ray fluorescent method for determination of total sulphur in bituminous coals

    International Nuclear Information System (INIS)

    Widowska-Kusmierska, J.; Siess, K.

    1979-01-01

    The X-ray fluorescent technique for the determination of total sulphur covering concentrations from 0,1 to 10% has been applied for bituminous coals showing a great variability in qualitative and quantitative composition of mineral matter (ash). The described method is a quick one giving results during one hour. The obtained good accuracy of determinations gives prospects for wide industrial application. (author)

  12. Dosimetry for total body irradiation of rhesus monkeys with 300 kV X- rays

    NARCIS (Netherlands)

    Zoetelief, J.; Wagemaker, G.; Broerse, J.J.

    1998-01-01

    Purpose: To obtain more accurate information on the dose distribution in rhesus monkeys for total body irradiation with orthovoltage X-rays. Materials and methods: Dose measurements were performed with an ionization chamber inside homogeneous cylindrical and rectangular phantoms of various

  13. Total chemical synthesis and X-ray structure of kaliotoxin by racemic protein crystallography.

    Science.gov (United States)

    Pentelute, Brad L; Mandal, Kalyaneswar; Gates, Zachary P; Sawaya, Michael R; Yeates, Todd O; Kent, Stephen B H

    2010-11-21

    Here we report the total synthesis of kaliotoxin by 'one pot' native chemical ligation of three synthetic peptides. A racemic mixture of D- and L-kaliotoxin synthetic protein molecules gave crystals in the centrosymmetric space group P1 that diffracted to atomic-resolution (0.95 Å), enabling the X-ray structure of kaliotoxin to be determined by direct methods.

  14. Self-consistent approach to x-ray reflection from rough surfaces

    International Nuclear Information System (INIS)

    Feranchuk, I. D.; Feranchuk, S. I.; Ulyanenkov, A. P.

    2007-01-01

    A self-consistent analytical approach for specular x-ray reflection from interfaces with transition layers [I. D. Feranchuk et al., Phys. Rev. B 67, 235417 (2003)] based on the distorted-wave Born approximation (DWBA) is used for the description of coherent and incoherent x-ray scattering from rough surfaces and interfaces. This approach takes into account the transformation of the modeling transition layer profile at the interface, which is caused by roughness correlations. The reflection coefficients for each DWBA order are directly calculated without phenomenological assumptions on their exponential decay at large scattering angles. Various regions of scattering angles are discussed, which show qualitatively different dependence of the reflection coefficient on the scattering angle. The experimental data are analyzed using the method developed

  15. Total reflection X-ray fluorescence applied to the chemical elements analysis of the mate tea infusion (Ilex-paraguariensis); Fluorescencia de raios-X por reflexao total aplicada a analise de elementos quimicos em cha de erva-mate (Ilex-paraguariensis)

    Energy Technology Data Exchange (ETDEWEB)

    Lopes, Fabio; Appoloni, Carlos R. [Universidade Estadual de Londrina, PR (Brazil). Lab. de Fisica Nuclear Aplicada; Cunha, Richard M. da Silva e; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear

    2002-07-01

    The purpose was to evaluate simultaneously the chemical element concentrations from K to Sr (19{<=}Z{<=}38) range in six samples of mate tea (Ilex paraguariensis) infusion, commercially available in Paraguay and South of Brazil. The chemical analysis of this beverage has a great nutritional importance for the native people of these areas, due to their large daily consumption. For the determination of these elements the dry-ashing and total reflection X-rays fluorescence (TXRF) were used. The methodology showed limits of detection among 81 ng.mL-1 for K to 10 ng.mL{sup -1} for Zn. Six infusion samples were prepared in triplicate, and the concentration was 3,8 to 10,2 {mu}g.mL{sup -1} for K, Ca and Mn, 0,21 to 1,07 {mu}g. mL{sup -1} for Fe and Zn and 0.03 to 0,17 {mu}g.mL{sup -1} for Ni, Cu, Br, Rb and Sr. The Mn and Ni concentrations are above the maximum permissible values for drinking water established by World Health Organization and Brazilian legislation (these organisms do not regulate the maximum permissible values for chemical elements in mate tea infusion). (author)

  16. X-ray reflection from cold matter in the nuclei of active galaxies

    International Nuclear Information System (INIS)

    Pounds, K.A.; Nandra, K.; Stewart, G.C.; George, I.M.; Fabian, A.C.

    1990-01-01

    The evidence accumulated over the past few years for strong soft X-ray emission from active galactic nuclei has been interpreted as black body emission from the innermost stable region of an accretion disk feeding the putative black hole at the centre of the active nucleus, a view given strong support by the rapid variability of some soft X-ray components. More recently, new X-ray data from the Exosat and Ginga satellites have revealed a second indicator of optically thick matter in the vicinity of the active nucleus, in the form of an iron K-fluorescence line at ≅ 6.4 keV. We report the discovery of two further common features of continuum absorption and reflection, revealed in a composite spectrum from twelve Ginga observations of Seyfert-type active galactic nuclei. Most of these spectral features are shown to be well modelled by reprocessing of the hard X-ray power-law continuum in a slab (or perhaps a disk) of cold matter. There is also evidence for a substantial line-of-sight column of photoionized material. (author)

  17. Density determination of langmuir-blodgett monolayer films using x-ray reflectivity technique

    International Nuclear Information System (INIS)

    Damar Yoga Kusuma

    2015-01-01

    Monolayer deposition by Langmuir-Blodgett technique produces monolayer films that are uniform with controllable thickness down to nanometer scale. To evaluate the quality of the monolayer deposition, X-ray reflectivity technique are employed to monitor the monolayers density. Langmuir-Blodgett monolayer with good coverage and uniformity results in film density close to its macroscopic film counterpart whereas films with presence of air gaps shows lower density compared to its macroscopic film counterpart. (author)

  18. Advanced analysis techniques for X-ray reflectivities. Theory and application

    International Nuclear Information System (INIS)

    Zimmermann, Klaus Martin

    2005-01-01

    The first part of this thesis adresses the phase problem in X-ray reflectivity. The analytical properties of the reflection coefficient imply that the phase is completely determined by the Hilbert transform of the logarithm of the modulus and the zeros in the upper half complex plane (UHP). To account in addition for interfacial roughness, a new formula for the Hilbert-phase is derived.In the following, the conditions for which the reflection coefficient has zeros in the UHP is discussed and the existing sufficient condition is extended to rough multi-layer systems. Procedures for locating these zeros are developed. The second part of this thesis introduces a new iterative inversion method for X-ray reflectivity. It expands the profile in a set of eigenfunctions, which are discrete approximations of the eigenfunction of the classical reconstruction problem of a compact supported function from its partially known Fourier-transform. In this work, piecewise constant functions, polygons and second-order B-splines are used to expand the density profile. The eigenvalue problems for the calculation of the above mentioned approximations are stated and solved. The formalism for the calculation of the reflection coefficient for these profiles is developed in dynamical and single-scattering theory. In the experimental part of this work iterative inverse schemes are applied to the analysis of X-ray reflectivity. Different sample systems are investigated: For two titanium-carbon samples tiny details at the Ti/C interface such as the formation of a thin TiC layer can be observed.The density profiles obtained from the reflectivities taken from nickel-carbon samples show the formation of SiC inside the Si sub strate. Finally, the new inversion scheme is applied to a series of reflectivities from a 700 AaSiGe film on a substrate.

  19. Advanced analysis techniques for X-ray reflectivities. Theory and application

    Energy Technology Data Exchange (ETDEWEB)

    Zimmermann, Klaus Martin

    2005-07-01

    The first part of this thesis adresses the phase problem in X-ray reflectivity. The analytical properties of the reflection coefficient imply that the phase is completely determined by the Hilbert transform of the logarithm of the modulus and the zeros in the upper half complex plane (UHP). To account in addition for interfacial roughness, a new formula for the Hilbert-phase is derived.In the following, the conditions for which the reflection coefficient has zeros in the UHP is discussed and the existing sufficient condition is extended to rough multi-layer systems. Procedures for locating these zeros are developed. The second part of this thesis introduces a new iterative inversion method for X-ray reflectivity. It expands the profile in a set of eigenfunctions, which are discrete approximations of the eigenfunction of the classical reconstruction problem of a compact supported function from its partially known Fourier-transform. In this work, piecewise constant functions, polygons and second-order B-splines are used to expand the density profile. The eigenvalue problems for the calculation of the above mentioned approximations are stated and solved. The formalism for the calculation of the reflection coefficient for these profiles is developed in dynamical and single-scattering theory. In the experimental part of this work iterative inverse schemes are applied to the analysis of X-ray reflectivity. Different sample systems are investigated: For two titanium-carbon samples tiny details at the Ti/C interface such as the formation of a thin TiC layer can be observed.The density profiles obtained from the reflectivities taken from nickel-carbon samples show the formation of SiC inside the Si sub strate. Finally, the new inversion scheme is applied to a series of reflectivities from a 700 AaSiGe film on a substrate.

  20. Numerical controlled diamond fly cutting machine for grazing incidence X-ray reflection mirrors

    International Nuclear Information System (INIS)

    Uchida, Fumihiko; Moriyama, Shigeo; Seya, Eiiti

    1992-01-01

    Synchrotron radiation has reached the stage of practical use, and the application to the wide fields that support future advanced technologies such as spectroscopy, the structural analysis of matters, semiconductor lithography and medical light source is expected. For the optical system of the equipment utilizing synchrotron radiation, the total reflection mirrors of oblique incidence are used for collimating and collecting X-ray. In order to restrain their optical aberration, nonspherical shape is required, and as the manufacturing method with high precision for nonspherical mirrors, a numerically controlled diamond cutting machine was developed. As for the cutting of soft metals with diamond tools, the high precision machining of any form can be done by numerical control, the machining time can be reduced as compared with grinding, and the cooling effect is large in metals. The construction of the cutting machine, the principle of machining, the control system, the method of calculating numerical control data, the investigation of machinable forms and the result of evaluation are reported. (K.I.)

  1. RASOR: an advanced instrument for soft x-ray reflectivity and diffraction.

    Science.gov (United States)

    Beale, T A W; Hase, T P A; Iida, T; Endo, K; Steadman, P; Marshall, A R; Dhesi, S S; van der Laan, G; Hatton, P D

    2010-07-01

    We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle (theta, 2theta, and chi) diffractometer with an additional removable rotation (phi) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorized motions are provided for the precise positioning of the sample onto the diffractometer center of rotation, and for positioning the center of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument.

  2. Non-Deforming, High-Reflectance X-ray Coatings for Lynx and Other Future Missions

    Science.gov (United States)

    Windt, David

    The overarching challenge addressed by this proposal is the development of highreflectance, high-resolution X-ray mirrors, to be used for the construction of lightweight X-ray telescopes for future NASA astronomy missions such as Lynx and others. The proposal's two specific aims are: 1) the development of optimized iridium-based interference coatings for the 0.1–10 keV band; and 2) the development of methods to mitigate coating-stress-induced substrate deformations in thin-shell glass and Si mirror segments. These goals will be achieved by building on established film deposition techniques and metrology infrastructure for X-ray optics that have been developed and advanced by the PI through APRA funding since 1999. Specific Aim #1: Interference Coatings for the 0.1–10 keV Energy Band Telescope effective area can be maximized by using Ir-based reflective coatings that exploit optical interference to provide higher reflectance than Ir alone. However, only preliminary investigations of such coatings have been conducted thus far; more research is required to fully optimize these coatings for maximum performance, to experimentally determine the coating designs that are feasible, and to determine the achievable X-ray reflectance, film stress, surface roughness, and thermal and temporal stability. The first specific aim of this proposal is to reach these very goals through a comprehensive research program. Demonstration of the achievable reflectance, stress, and roughness in stable, optimized coatings will in turn facilitate global telescope design optimization, by identifying the best coating for each mirror shell based on incidence angle, and on telescope effective-area and field-of-view requirements. The research has the potential to greatly increase the effective area of future X-ray telescopes. Specific Aim #2: Mitigation of Coating-Stress-Induced Substrate Deformations High-quality films of Ir and other candidate materials (e.g., B4C) to be investigated for the 0

  3. The reflected amplitude ratio of multilayers and superlattice describe the dynamical diffraction of x-rays

    International Nuclear Information System (INIS)

    Bhatti, Q.A.; Mangi, F.A.

    2006-01-01

    Calculating the rocking curves of complicated layered structures, such as non-ideal super lattices on perfect crystals are clearly exposed with observed diffraction profile. Recursion formulas for calculating reflected amplitude ratio of multilayer and super lattices have been involved from the Takagi-Taupin differential equation, which describes the dynamical diffraction of X-rays in deformed crystal. The Kinematical theory can computing time only in case of ideal superlattice for which geometric series can be used but the reflectivity must be below 10 % so that multiple reflections can be neglected for a perfect crystal of arbitrary thickness the absorption at the centre of the dynamical reflection is found to be proportional to the square root of the reflectivity. Sputter- deposited periodic multilayers of tungsten and carbon can be considered as an artificial crystal, for which dynamical X-rays diffraction calculations give the result very similar to those of macroscopic optical description in terms of the complex index of refraction and Frensnel relation coefficient. (author)

  4. Capabilities of using white x-rays for the reconstruction of surface morphology from coherent reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Sant, Tushar, E-mail: tushar@physik.uni-siegen.de [Solid State Physics Group, University of Siegen, 57068 Siegen (Germany); Panzner, Tobias [Paul Scherrer Institute (Switzerland); Pietsch, Ullrich [Solid State Physics Group, University of Siegen, 57068 Siegen (Germany)

    2010-10-15

    We present a new method to reconstruct the surface profile of a sample from coherent reflectivity data of a white x-ray beam experiment. As an example the surface profile of a laterally confined silicon wafer has been reconstructed quantitatively from static speckle measurements using white coherent x-rays from a bending magnet in the energy range between 5 < E < 20 keV. As a consequence of using white radiation, speckles appear in addition to the Airy pattern caused by scattering at the entrance pinhole. Nevertheless, the surface profile of a triangularly shaped specimen was reconstructed considering sufficient oversampling between the beam-footprint and the effective sample width. For the profile reconstruction the Error-Reduction phase retrieval algorithm was modified by including the spectral illumination function and a Fresnel propagator term. The simultaneous use of different x-ray energies having different penetration depth provides information on the evolution of the surface profile from the near-surface towards the bulk. The limitations of present experiment can be overcome using white or pink radiation from a source with higher photon flux.

  5. Analysis of biological slurry samples by total x-ray fluorescence after in situ microwave digestion

    International Nuclear Information System (INIS)

    Lue-Meru, M.P.; Capote, T.; Greaves, E.

    2000-01-01

    Biological slurry samples were analyzed by total reflection x-ray fluorescence (TXRF) after an in situ microwave digestion procedure on the quartz reflector. This method lead to the removal of the matrix by the digestion and permits the enrichment of the analites by using sample amounts higher than those normally used in TXRF for the thin layer requirement since the organic matrix is removed. In consequence, the pre-concentration of sample is performed and the detection capability is increased by a quasi direct method. The samples analyzed were the international IAEA blood standard, the SRM bovine liver 1577-a standard and fresh onion tissues. Slurries were prepared in three ways: a.- weighing a sample amount on the reflector and adding suprapure nitric acid and internal standard followed by microwave digestion, b.-weighing a sample amount and water with an appropriate concentration of the internal standard in an Eppendorf vial, taking then an aliquot to the quartz reflector for microwave digestion with suprapure nitric acid, c.- weighing a sample amount of fresh tissue, homogenising with high speed homegenator to obtain a slurry sample which can be diluted in an ependorf vial with water an the internal standard. Then an aliquot is taken to the reflector for microwave digestion with suprapure nitric acid. Further details of sample preparation procedures will be discussed during presentation. The analysis was carried out in a Canberra spectrometer using the Kalpha lines of the Ag and Mo tubes. The elements Ca, K, Fe, Cu, Zn, Se, Mn, Rb, Br, Sr were determined. The effect of the preparation procedure was evaluated by the accuracy and precision of the results for each element and the percent of recovery. (author)

  6. Use of overlapped reflection for determining the retained austenite by X-ray diffraction

    International Nuclear Information System (INIS)

    Garin, J.L.; Gonzalez, C.F.

    1988-01-01

    Retainec austenite in high-carbon steels has been determined by means of new computation techniques applied to the processing of X-ray diffraction data. Instead of using the traditional procedure based on the weak (200) reflections of martensite and austenite, intensity measurements of the overlapped (110) peak of martensite and (111) peak of austenite were performed. The separation of the peaks was based on a Pearson VII function, which is capable of describing all diffraction profiles. The accuracy of integrated intensities was then improved with the beneficial effects of higher precision in the calculation of the amount of retained austenite. (author) [pt

  7. Structure of ordered polyelectrolyte films from atomic-force microscopy and X-ray reflectivity data

    International Nuclear Information System (INIS)

    Belyaev, V.V.; Tolstikhina, A.L.; Stepina, N.D.; Kayushina, R.L.

    1998-01-01

    The possible application of atomic-force microscopy and X-ray reflectometry methods to structural studies of polyelectrolyte films obtained due to alternating adsorption of oppositely charged polyanion [sodium polysterenesulfonate (PSS)] and polycation [poly(allylamine) hydrochloride (PAA)] layers on solid substrates has been considered. The atomic-force microscopy study has revealed the characteristic features of the surface topography of samples consisting of different numbers of polyelectrolyte layers deposited from solutions characterized by different ionic strength values. It is shown that the shape of the reflectivity curves obtained from thin polyelectrolyte films depends on their surface structure

  8. Testing the Performance and Accuracy of the RELXILL Model for the Relativistic X-Ray Reflection from Accretion Disks

    Science.gov (United States)

    Choudhury, Kishalay; García, Javier A.; Steiner, James F.; Bambi, Cosimo

    2017-12-01

    The reflection spectroscopic model RELXILL is commonly implemented in studying relativistic X-ray reflection from accretion disks around black holes. We present a systematic study of the model’s capability to constrain the dimensionless spin and ionization parameters from ∼6000 Nuclear Spectroscopic Telescope Array (NuSTAR) simulations of a bright X-ray source employing the lamp-post geometry. We employ high-count spectra to show the limitations in the model without being confused with limitations in signal-to-noise. We find that both parameters are well-recovered at 90% confidence with improving constraints at higher reflection fraction, high spin, and low source height. We test spectra across a broad range—first at 106–107 and then ∼105 total source counts across the effective 3–79 keV band of NuSTAR, and discover a strong dependence of the results on how fits are performed around the starting parameters, owing to the complexity of the model itself. A blind fit chosen over an approach that carries some estimates of the actual parameter values can lead to significantly worse recovery of model parameters. We further stress the importance to span the space of nonlinear-behaving parameters like {log} ξ carefully and thoroughly for the model to avoid misleading results. In light of selecting fitting procedures, we recall the necessity to pay attention to the choice of data binning and fit statistics used to test the goodness of fit by demonstrating the effect on the photon index Γ. We re-emphasize and implore the need to account for the detector resolution while binning X-ray data and using Poisson fit statistics instead while analyzing Poissonian data.

  9. In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1{sub 0} ordering in {sup 57}Fe/Pt multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore-452 017 (India); Leitenberger, Wolfram [Institute of Physics, University of Potsdam, 14469 Potsdam (Germany); Pietsch, U [Physics Department, University of Siegen, D-57068 Siegen (Germany)], E-mail: vrreddy@csr.ernet.in, E-mail: varimalla@yahoo.com

    2009-05-06

    In situ high temperature x-ray reflectivity and grazing incidence x-ray diffraction measurements in the energy dispersive mode are used to study the ordered face-centered tetragonal (fct) L 1{sub 0} phase formation in [Fe(19 A)/Pt(25 A)]{sub x 10} multilayers prepared by ion beam sputtering. With the in situ x-ray measurements it is observed that (i) the multilayer structure first transforms to a disordered FePt and subsequently to an ordered fct L 1{sub 0} phase, (ii) the ordered fct L 1{sub 0} FePt peaks start to appear at 320 deg. C annealing, (iii) the activation energy of the interdiffusion is 0.8 eV and (iv) ordered fct FePt grains have preferential out-of-plane texture. The magneto-optical Kerr effect and conversion electron Moessbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 deg. C annealed multilayers. The magnetic data for the 400 {sup 0}C annealed sample indicate that the magnetization is at an angle of {approx}50 deg. from the plane of the film.

  10. Full Polarization Analysis of Resonant Superlattice and Forbidden x-ray Reflections in Magnetite

    International Nuclear Information System (INIS)

    Wilkins, S.B.; Bland, S.R.; Detlefs, B.; Beale, T.A.W.; Mazzoli, C.; Joly, Y.; Hatton, P.D.; Lorenzo, J.E.; Brabers, V.A.M.

    2009-01-01

    Despite being one of the oldest known magnetic materials, and the classic mixed valence compound, thought to be charge ordered, the structure of magnetite below the Verwey transition is complex and the presence and role of charge order is still being debated. Here, we present resonant x-ray diffraction data at the iron K-edge on forbidden (0, 0, 2n+1) C and superlattice (0, 0, 2n+1/2)C reflections. Full linear polarization analysis of the incident and scattered light was conducted in order to explore the origins of the reflections. Through simulation of the resonant spectra we have confirmed that a degree of charge ordering takes place, while the anisotropic tensor of susceptibility scattering is responsible for the superlattice reflections below the Verwey transition. We also report the surprising result of the conversion of a significant proportion of the scattered light from linear to nonlinear polarization.

  11. Combining mid infrared and total X-ray fluorescence spectroscopy for prediction of soil properties

    Science.gov (United States)

    Towett, Erick; Shepherd, Keith; Sila, Andrew; Aynekulu, Ermias; Cadisch, Georg

    2015-04-01

    Mid-infrared diffuse reflectance spectroscopy (MIR) can predict many soil properties but extractable nutrients are often predicted poorly. We evaluated the potential of MIR and total elemental analysis using total X-ray fluorescence spectroscopy (TXRF), both individually and combined, to predict results of conventional soil tests. Total multi-elemental analysis provides a fingerprint of soil mineralogy and could predict some soil properties and help improve MIR predictions. A set of 700 georeferenced soil samples associated with the Africa Soil Information Service (AfSIS) (www.africasoils.net) from 44 stratified randomly-located 100-km2 sentinel sites distributed across sub-Saharan Africa were analysed for physico-chemical composition using conventional reference methods, and compared to MIR and TXRF spectra using the Random Forests regression algorithm and an internal out-of-bag validation. MIR spectra resulted in good prediction models (R2 >0.80) for organic C and total N, Mehlich-3 Ca and Al, and pH. To test the combined spectroscopic approach, TXRF element concentration data was included as a property predictor along with the first derivative of MIR spectral data using the RF algorithm. Including TXRF did not improve prediction of these properties. TXRF was poorer (R2 0.86) as these elements are not directly determined with TXRF, however the variance explained is still quite high and may be attributable to TXRF signatures relating to mineralogy correlated with protection of soil organic matter. TXRF model for Mehlich-3 Al had excellent prediction capability explaining 81% of the observed variation in extractable Al content and was comparable to that of MIR (R2 = 0.86). However, models for pH and Mehlich-3 exchangeable Ca exhibited R2 values of 0.74 and 0.79 respectively and thus had moderate predictive accuracy, compared to MIR alone with R2 values of 0.82 and 0.84 respectively. Both MIR and TXRF methods predicted soil properties that relate to nutrient

  12. Determining surface coverage of ultra-thin gold films from X-ray reflectivity measurements

    International Nuclear Information System (INIS)

    Kossoy, A.; Simakov, D.; Olafsson, S.; Leosson, K.

    2013-01-01

    The paper describes usage of X-ray reflectivity for characterization of surface coverage (i.e. film continuity) of ultra-thin gold films which are widely studied for optical, plasmonic and electronic applications. The demonstrated method is very sensitive and can be applied for layers below 1 nm. It has several advantages over other techniques which are often employed in characterization of ultra-thin metal films, such as optical absorption, Atomic Force Microscopy, Transmission Electron Microscopy or Scanning Electron Microscopy. In contrast to those techniques our method does not require specialized sample preparation and measurement process is insensitive to electrostatic charge and/or presence of surface absorbed water. We validate our results with image processing of Scanning Electron Microscopy images. To ensure precise quantitative analysis of the images we developed a generic local thresholding algorithm which allowed us to treat series of images with various values of surface coverage with similar image processing parameters. - Highlights: • Surface coverage/continuity of ultra-thin Au films (up to 7 nm) was determined. • Results from X-ray reflectivity were verified by scanning electron microscopy. • We developed local thresholding algorithm to treat non-homogeneous image contrast

  13. Probing Ultrafast Electron Dynamics at Surfaces Using Soft X-Ray Transient Reflectivity Spectroscopy

    Science.gov (United States)

    Baker, L. Robert; Husek, Jakub; Biswas, Somnath; Cirri, Anthony

    The ability to probe electron dynamics with surface sensitivity on the ultrafast time scale is critical for understanding processes such as charge separation, injection, and surface trapping that mediate efficiency in catalytic and energy conversion materials. Toward this goal, we have developed a high harmonic generation (HHG) light source for femtosecond soft x-ray reflectivity. Using this light source we investigated the ultrafast carrier dynamics at the surface of single crystalline α-Fe2O3, polycrystalline α-Fe2O3, and the mixed metal oxide, CuFeO2. We have recently demonstrated that CuFeO2 in particular is a selective catalyst for photo-electrochemical CO2 reduction to acetate; however, the role of electronic structure and charge carrier dynamics in mediating catalytic selectivity has not been well understood. Soft x-ray reflectivity measurements probe the M2,3, edges of the 3d transition metals, which provide oxidation and spin state resolution with element specificity. In addition to chemical state specificity, these measurements are also surface sensitive, and by independently simulating the contributions of the real and imaginary components of the complex refractive index, we can differentiate between surface and sub-surface contributions to the excited state spectrum. Accordingly, this work demonstrates the ability to probe ultrafast carrier dynamics in catalytic materials with element and chemical state specificity and with surface sensitivity.

  14. Synchrotron x-ray reflectivity study of oxidation/passivation of copper and silicon

    International Nuclear Information System (INIS)

    Chu, Y.; Nagy, Z.; Parkhutik, V.; You, H.

    1999-01-01

    Synchrotron x-ray-scattering technique studies of copper and silicon electrochemical interfaces are reported. These two examples illustrate the application of synchrotron x-ray techniques for oxidation, passivation, and dissolution of metals and semiconductors

  15. Synchrotron x-ray reflectivity study of oxidation/passivation of copper and silicon.

    Energy Technology Data Exchange (ETDEWEB)

    Chu, Y.; Nagy, Z.; Parkhutik, V.; You, H.

    1999-07-21

    Synchrotron x-ray-scattering technique studies of copper and silicon electrochemical interfaces are reported. These two examples illustrate the application of synchrotron x-ray techniques for oxidation, passivation, and dissolution of metals and semiconductors.

  16. Application of total reflection X-ray fluorescence spectrometry for ...

    Indian Academy of Sciences (India)

    terest because of the increased awareness about environmental pollution and human health as some ... The presence of heavy elements indicates .... technique applicable to metals and nonmetals equally, both metals and nonmetals present.

  17. Total reflection X-ray fluorescence and energy-dispersive X-ray ...

    Indian Academy of Sciences (India)

    Nuclear energy is one of the clean options of electricity generation for the betterment of human life. India has an ambitious program for such electricity generation using different types of nuclear reactors. The safe and efficient generation of electricity from these reactors requires quality control of different nuclear materials, ...

  18. Total reflection X-ray fluorescence and energy-dispersive X-ray ...

    Indian Academy of Sciences (India)

    (ICP-AES), atomic absorption spectrometry (AAS) and spark source mass spectrome- ... actinide oxides, for trace element determinations normal XRF cannot ... at a flat polished sample support at an angle less than the critical angle and thus ...

  19. High Reflectance Nanoscale V/Sc Multilayer for Soft X-ray Water Window Region.

    Science.gov (United States)

    Huang, Qiushi; Yi, Qiang; Cao, Zhaodong; Qi, Runze; Loch, Rolf A; Jonnard, Philippe; Wu, Meiyi; Giglia, Angelo; Li, Wenbin; Louis, Eric; Bijkerk, Fred; Zhang, Zhong; Wang, Zhanshan

    2017-10-10

    V/Sc multilayer is experimentally demonstrated for the first time as a high reflectance mirror for the soft X-ray water window region. It primarily works at above the Sc-L edge (λ = 3.11 nm) under near normal incidence while a second peak appears at above the V-L edge (λ = 2.42 nm) under grazing incidence. The V/Sc multilayer fabricated with a d-spacing of 1.59 nm and 30 bilayers has a smaller interface width (σ = 0.27 and 0.32 nm) than the conventional used Cr/Sc (σ = 0.28 and 0.47 nm). For V/Sc multilayer with 30 bilayers, the introduction of B 4 C barrier layers has little improvement on the interface structure. As the number of bilayers increasing to 400, the growth morphology and microstructure of the V/Sc layers evolves with slightly increased crystallization. Nevertheless, the surface roughness remains to be 0.25 nm. A maximum soft X-ray reflectance of 18.4% is measured at λ = 3.129 nm at 9° off-normal incidence using the 400-bilayers V/Sc multilayer. According to the fitted model, an s-polarization reflectance of 5.2% can also be expected at λ = 2.425 nm under 40° incidence. Based on the promising experimental results, further improvement of the reflectance can be achieved by using a more stable deposition system, exploring different interface engineering methods and so on.

  20. A high resolution reflecting crystal spectrometer to measure 3 keV pionic hydrogen and deuterium X-rays

    International Nuclear Information System (INIS)

    Badertscher, A.; Bogdan, M.; Goudsmit, P.F.A.; Knecht, L.; Leisi, H.J.; Schroeder, H.C.; Sigg, D.; Zhao, Z.G.; Chatellard, D.; Egger, J.P.; Jeannet, E.; Aschenauer, E.C.; Gabathuler, K.; Simons, L.M.; Rusi El Hassani, A.J.

    1993-01-01

    A reflecting crystal spectrometer consisting of three cylindrically bent quartz (110) crystals is described. It was designed to measure the 3 keV K β X-rays from pionic hydrogen and deuterium. Charge coupled devices (CCDs) were used as X-ray detectors. Projecting the reflexes of all three crystals on one common focus, an instrumental energy resolution below 1 eV was obtained at an energy of 2.9 keV. (orig.)

  1. Recent Developments in the X-Ray Reflectivity Analysis for Rough Surfaces and Interfaces of Multilayered Thin Film Materials

    Directory of Open Access Journals (Sweden)

    Yoshikazu Fujii

    2013-01-01

    Full Text Available X-ray reflectometry is a powerful tool for investigations on rough surface and interface structures of multilayered thin film materials. The X-ray reflectivity has been calculated based on the Parratt formalism, accounting for the effect of roughness by the theory of Nevot-Croce conventionally. However, in previous studies, the calculations of the X-ray reflectivity often show a strange effect where interference effects would increase at a rough surface. And estimated surface and interface roughnesses from the X-ray reflectivity measurements did not correspond to the TEM image observation results. The strange result had its origin in a used equation due to a serious mistake in which the Fresnel transmission coefficient in the reflectivity equation is increased at a rough interface because of a lack of consideration of diffuse scattering. In this review, a new accurate formalism that corrects this mistake is presented. The new accurate formalism derives an accurate analysis of the X-ray reflectivity from a multilayer surface of thin film materials, taking into account the effect of roughness-induced diffuse scattering. The calculated reflectivity by this accurate reflectivity equation should enable the structure of buried interfaces to be analyzed more accurately.

  2. Soft X-ray reflectivity: from quasi-perfect mirrors to accelerator walls

    CERN Document Server

    Schäfers, F.

    2013-04-22

    Reflection of light from surfaces is a very common, but complex phenomenon not only in science and technology, but in every day life. The underlying basic optical principles have been developed within the last five centuries using visible light available from the sun or other laboratory light sources. X-rays were detected in 1895, and the full potential of soft- and hard-x ray radiation as a probe for the electronic and geometric properties of matter, for material analysis and its characterisation is available only since the advent of synchrotron radiation sources some 50 years ago. On the other hand high-brilliance and high power synchrotron radiation of present-days 3rd and 4th generation light sources is not always beneficial. Highenergy machines and accelerator-based light sources can suffer from a serious performance drop or limitations due to interaction of the synchrotron radiation with the accelerator walls, thus producing clouds of photoelectrons (e-cloud) which in turn interact with the accelerated ...

  3. Revisiting the total ion yield x-ray absorption spectra of liquid water microjets

    International Nuclear Information System (INIS)

    Saykally, Richard J; Cappa, Chris D.; Smith, Jared D.; Wilson, Kevin R.; Saykally, Richard J.

    2008-01-01

    Measurements of the total ion yield (TIY) x-ray absorption spectrum (XAS) of liquid water by Wilson et al. (2002 J. Phys.: Condens. Matter 14 L221 and 2001 J. Phys. Chem. B 105 3346) have been revisited in light of new experimental and theoretical efforts by our group. Previously, the TIY spectrum was interpreted as a distinct measure of the electronic structure of the liquid water surface. However, our new results indicate that the previously obtained spectrum may have suffered from as yet unidentified experimental artifacts. Although computational results indicate that the liquid water surface should exhibit a TIY-XAS that is fundamentally distinguishable from the bulk liquid XAS, the new experimental results suggest that the observable TIY-XAS is actually nearly identical in appearance to the total electron yield (TEY-)XAS, which is a bulk probe. This surprising similarity between the observed TIY-XAS and TEY-XAS likely results from large contributions from x-ray induced electron stimulated desorption of ions, and does not necessarily indicate that the electronic structure of the bulk liquid and liquid surface are identical

  4. REX - a program for the analysis of X-ray reflectivity data: user guide and programmer manual

    International Nuclear Information System (INIS)

    Crabb, T.A.; Gibson, P.N.

    1992-12-01

    A FORTRAN program REX, which has been developed to facilitate the interpretation of X-ray reflectivity data, is described. The program allows the simulation of reflectivity profiles as a function of either incident angle or of energy. Factors such as anomalous dispersion, and surface and interface roughness are taken into account in the model. In addition, experimental data of reflectivity as a function of incident angle can be matched to user-supplied theoretical parameters by a least-squares refinement procedure. Experimental reflectivity data recorded at several X-ray wavelengths can be analysed simultaneously, thus eliminating certain experimental errors. (author)

  5. The X-ray reflectivity of the AXAF VETA-I optics

    Science.gov (United States)

    Kellogg, E.; Chartas, G.; Graessle, D.; Hughes, J. P.; Van Speybroeck, L.; Zhao, Ping; Weisskopf, M. C.; Elsner, R. F.; O'Dell, S. L.

    1993-01-01

    The study measures the X-ray reflectivity of the AXAF VETA-I optic and compares it with theoretical predictions. Measurements made at energies of 0.28, 0.9, 1.5, 2.1, and 2.3 keV are compared with predictions based on ray trace calculations. Results on the variation of the reflectivity with energy as well as the absolute value of the reflectivity are presented. A synchrotron reflectivity measurement with a high-energy resolution over the range 0.26 to 1.8 keV on a flat Zerodur sample is also reported. Evidence is found for contamination of the flat by a thin layer of carbon on the surface, and the possibility of alteration of the surface composition of the VETA-I mirror, perhaps by the polishing technique. The overall agreement between the measured and calculated effective area of VETA-I is between 2.6 and 10 percent. Measurements at individual energies deviate from the best-fitting calculation to 0.3 to 0.8 percent, averaging 0.6 percent at energies below the high energy cutoff of the mirror reflectivity, and are as high as 20.7 percent at the cutoff.

  6. Improved analytical formulas for x-ray and neutron reflection from surface films

    International Nuclear Information System (INIS)

    Zhou, X.; Chen, S.; Felcher, G.P.

    1992-01-01

    A general and exact expression for x-ray and neutron reflectance and transmittance is given in terms of an integral of the real-space scattering-length-density profile fluctuation of the film, with respect to an arbitrary constant reference density level, over the wave function inside the film. Various special cases and approximations are then derived from this exact form by suitable approximations of the wave function. In particular, two practical approximate formulas are derived which are improvement over the corresponding distorted-wave Born approximations. One is for an arbitrary film deposited on a known substrate and the other for a free liquid surface. Numerical results are used to illustrate the accuracy of these formulas

  7. Observation on Surface Change of Fragile Glass: Temperature - Time Dependence Studied by X-Ray Reflectivity

    International Nuclear Information System (INIS)

    Kikkawa, Hiroyuki; Kitahara, Amane; Takahashi, Isao

    2004-01-01

    The structural change of a fragile glass surface close to the glass transition temperature Tg is studied by using X-ray reflectivity. Measurements were performed on surfaces of maltitol, which is a typical polyalcohol fragile glass with Tg = 320K. Upon both heating and cooling, we find the following features which are also noticed in silicate glass surfaces: (i) On heating, the surface morphology indicates a variation at temperatures below Tg; (ii) A drastic increase in surface roughness occurs at a temperature about 333K on heating, which is 13K higher than Tg; (iii) During the cooling of the sample, formation of a low-density surface layer (3nm at 293K) is observed. Prior to the crystallization, nm - μm sized domains were grown at the surface, which might not be reported for other glasses

  8. Chromatic X-ray magnifying method and apparatus by Bragg reflective planes on the surface of Abbe sphere

    Science.gov (United States)

    Thoe, Robert S.

    1991-01-01

    Method and apparatus for producing sharp, chromatic, magnified images of X-ray emitting objects, are provided. The apparatus, which constitutes an X-ray microscope or telescope, comprises a connected collection of Bragg reflecting planes, comprised of either a bent crystal or a synthetic multilayer structure, disposed on and adjacent to a locus determined by a spherical surface. The individual Bragg planes are spatially oriented to Bragg reflect radiation from the object location toward the image location. This is accomplished by making the Bragg planes spatially coincident with the surfaces of either a nested series of prolate ellipsoids of revolution, or a nested series of spheres. The spacing between the Bragg reflecting planes can be tailored to control the wavelengths and the amount of the X-radiation that is Bragg reflected to form the X-ray image.

  9. Effect of FEL induced ionization on X-ray reflectivity of multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Ksenzov, Dmitriy; Grigorian, Souren; Pietsch, Ullrich [University of Siegen (Germany)

    2009-07-01

    The VUV-FEL in Hamburg (FLASH) emits short-pulse radiation with wavelengths from 6 to 30 nm and a pulse length of 10-50 fs. The FLASH wavelength allows x-ray diffraction experiments at periodical multilayer's structures acting as 1D crystal. The probe of depth selective interaction of the high-intense x-ray short pulse with these objects can be used to obtain information about possible electronic excitation and various recombination processes inside multilayers. As known from recent experiments at FLASH, the later ones are most likely using highly intense FEL radiation. The ML reflectivity is analyzed for case of that the optical parameters are changing as function of the depth of the penetrating incident pulse into the multilayer. The response is studied for the model system La/B{sub 4}C using two experimental conditions both at fixed incidence angle: 1) the energy of the incident pulses, E, coincides with the energy of the 1st order multilayer Bragg peak, E{sub B}, of the reflection curve, and 2) the energy of incident pulse differs by a small dE from E{sub B}. The ML response to a given sub-pulse differs for both conditions. However, there is a clear fingerprint of ionization for both conditions for the case that E is close to the K-absorption edge of B-atoms. Our results support respective efforts to measure the optical parameters of solids under high-intense FEL radiation.

  10. STRONGER REFLECTION FROM BLACK HOLE ACCRETION DISKS IN SOFT X-RAY STATES

    International Nuclear Information System (INIS)

    Steiner, James F.; Remillard, Ronald A.; García, Javier A.; McClintock, Jeffrey E.

    2016-01-01

    We analyze 15,000 spectra of 29 stellar-mass black hole (BH) candidates collected over the 16 year mission lifetime of Rossi X-ray Timing Explorer using a simple phenomenological model. As these BHs vary widely in luminosity and progress through a sequence of spectral states, which we broadly refer to as hard and soft, we focus on two spectral components: the Compton power law and the reflection spectrum it generates by illuminating the accretion disk. Our proxy for the strength of reflection is the equivalent width of the Fe–K line as measured with respect to the power law. A key distinction of our work is that for all states we estimate the continuum under the line by excluding the thermal disk component and using only the component that is responsible for fluorescing the Fe–K line, namely, the Compton power law. We find that reflection is several times more pronounced (∼3) in soft compared to hard spectral states. This is most readily caused by the dilution of the Fe line amplitude from Compton scattering in the corona, which has a higher optical depth in hard states. Alternatively, this could be explained by a more compact corona in soft (compared to hard) states, which would result in a higher reflection fraction.

  11. STRONGER REFLECTION FROM BLACK HOLE ACCRETION DISKS IN SOFT X-RAY STATES

    Energy Technology Data Exchange (ETDEWEB)

    Steiner, James F.; Remillard, Ronald A. [MIT Kavli Institute for Astrophysics and Space Research, MIT, 70 Vassar Street, Cambridge, MA 02139 (United States); García, Javier A.; McClintock, Jeffrey E., E-mail: jsteiner@mit.edu [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge, MA 02138 (United States)

    2016-10-01

    We analyze 15,000 spectra of 29 stellar-mass black hole (BH) candidates collected over the 16 year mission lifetime of Rossi X-ray Timing Explorer using a simple phenomenological model. As these BHs vary widely in luminosity and progress through a sequence of spectral states, which we broadly refer to as hard and soft, we focus on two spectral components: the Compton power law and the reflection spectrum it generates by illuminating the accretion disk. Our proxy for the strength of reflection is the equivalent width of the Fe–K line as measured with respect to the power law. A key distinction of our work is that for all states we estimate the continuum under the line by excluding the thermal disk component and using only the component that is responsible for fluorescing the Fe–K line, namely, the Compton power law. We find that reflection is several times more pronounced (∼3) in soft compared to hard spectral states. This is most readily caused by the dilution of the Fe line amplitude from Compton scattering in the corona, which has a higher optical depth in hard states. Alternatively, this could be explained by a more compact corona in soft (compared to hard) states, which would result in a higher reflection fraction.

  12. NuSTAR SPECTROSCOPY OF MULTI-COMPONENT X-RAY REFLECTION FROM NGC 1068

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Franz E. [Pontificia Universidad Católica de Chile, Instituto de Astrofísica, Casilla 306, Santiago 22 (Chile); Arévalo, Patricia [EMBIGGEN Anillo, Concepción (Chile); Walton, Dominic J.; Baloković, Mislav; Brightman, Murray; Harrison, Fiona A. [Cahill Center for Astronomy and Astrophysics, California Institute of Technology, Pasadena, CA 91125 (United States); Koss, Michael J. [Institute for Astronomy, Department of Physics, ETH Zurich, Wolfgang-Pauli-Strasse 27, CH-8093 Zurich (Switzerland); Puccetti, Simonetta [ASDC-ASI, Via del Politecnico, I-00133 Roma (Italy); Gandhi, Poshak [School of Physics and Astronomy, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom); Stern, Daniel [Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, Pasadena, CA 91109 (United States); Alexander, David M.; Moro, Agnese Del [Department of Physics, Durham University, South Road, Durham, DH1 3LE (United Kingdom); Boggs, Steve E.; Craig, William W. [Space Sciences Laboratory, University of California, Berkeley, CA 94720 (United States); Brandt, William N.; Luo, Bin [Department of Astronomy and Astrophysics, The Pennsylvania State University, 525 Davey Lab, University Park, PA 16802 (United States); Christensen, Finn E. [DTU Space, National Space Institute, Technical University of Denmark, Elektrovej 327, DK-2800 Lyngby (Denmark); Comastri, Andrea [INAF-Osservatorio Astronomico di Bologna, via Ranzani 1, I-40127 Bologna (Italy); Hailey, Charles J. [Columbia Astrophysics Laboratory, Columbia University, New York, NY 10027 (United States); Hickox, Ryan [Department of Physics and Astronomy, Dartmouth College, 6127 Wilder Laboratory, Hanover, NH 03755 (United States); and others

    2015-10-20

    We report on high-energy X-ray observations of the Compton-thick Seyfert 2 galaxy NGC 1068 with NuSTAR, which provide the best constraints to date on its >10 keV spectral shape. The NuSTAR data are consistent with those from past and current instruments to within cross-calibration uncertainties, and we find no strong continuum or line variability over the past two decades, which is in line with its X-ray classification as a reflection-dominated Compton-thick active galactic nucleus. The combined NuSTAR, Chandra, XMM-Newton, and Swift BAT spectral data set offers new insights into the complex secondary emission seen instead of the completely obscured transmitted nuclear continuum. The critical combination of the high signal-to-noise NuSTAR data and the decomposition of the nuclear and extranuclear emission with Chandra allow us to break several model degeneracies and greatly aid physical interpretation. When modeled as a monolithic (i.e., a single N{sub H}) reflector, none of the common Compton reflection models are able to match the neutral fluorescence lines and broad spectral shape of the Compton reflection hump without requiring unrealistic physical parameters (e.g., large Fe overabundances, inconsistent viewing angles, or poor fits to the spatially resolved spectra). A multi-component reflector with three distinct column densities (e.g., with best-fit values of N{sub H} of 1.4 × 10{sup 23}, 5.0 × 10{sup 24}, and 10{sup 25} cm{sup −2}) provides a more reasonable fit to the spectral lines and Compton hump, with near-solar Fe abundances. In this model, the higher N{sub H} component provides the bulk of the flux to the Compton hump, while the lower N{sub H} component produces much of the line emission, effectively decoupling two key features of Compton reflection. We find that ≈30% of the neutral Fe Kα line flux arises from >2″ (≈140 pc) and is clearly extended, implying that a significant fraction (and perhaps most) of the <10 keV reflected component

  13. Total radiation dosage from X-ray examinations in rheumatoid arthritis and other chronic skeletal diseases

    International Nuclear Information System (INIS)

    Baldursson, H.; Gustafsson, M.

    1977-01-01

    Young patients with rheumatoid arthritis and other chronic diseases of the skeleton are increasingly being operated on with replacement of major joints. The great number of associated X-ray examinations performed on these patients has caused some anxiety amongst orthopaedic surgeons. Two patients with juvenile rheumatoid arthritis have been studied. An attempt was made to calculate the total radiation dose to bone marrow and gonads. For lack of recommendations for the maximum permissible radiation dose to patients, the dose calculated has been compared with the maximum permissible dose of radiation workers, and with the dose limit for non-occupational irradiation of individuals. The yearly absorbed dose in these two patients is much lower than the maximum permissible dose of radiation workers and only slightly higher than the dose limit for non-occupational exposure of individuals. (author)

  14. Self-assembled iron oxide nanoparticle multilayer: x-ray and polarized neutron reflectivity

    International Nuclear Information System (INIS)

    Mishra, D; Benitez, M J; Petracic, O; Badini Confalonieri, G A; Szary, P; Brüssing, F; Devishvili, A; Toperverg, B P; Zabel, H; Theis-Bröhl, K; Vorobiev, A; Konovalov, O; Paulus, M; Sternemann, C

    2012-01-01

    We have investigated the structure and magnetism of self-assembled, 20 nm diameter iron oxide nanoparticles covered by an oleic acid shell for scrutinizing their structural and magnetic correlations. The nanoparticles were spin-coated on an Si substrate as a single monolayer and as a stack of 5 ML forming a multilayer. X-ray scattering (reflectivity and grazing incidence small-angle scattering) confirms high in-plane hexagonal correlation and a good layering property of the nanoparticles. Using polarized neutron reflectivity we have also determined the long range magnetic correlations parallel and perpendicular to the layers in addition to the structural ones. In a field of 5 kOe we determine a magnetization value of about 80% of the saturation value. At remanence the global magnetization is close to zero. However, polarized neutron reflectivity reveals the existence of regions in which magnetic moments of nanoparticles are well aligned, while losing order over longer distances. These findings confirm that in the nanoparticle assembly the magnetic dipole–dipole interaction is rather strong, dominating the collective magnetic properties at room temperature. (paper)

  15. Self-assembled iron oxide nanoparticle multilayer: x-ray and polarized neutron reflectivity.

    Science.gov (United States)

    Mishra, D; Benitez, M J; Petracic, O; Badini Confalonieri, G A; Szary, P; Brüssing, F; Theis-Bröhl, K; Devishvili, A; Vorobiev, A; Konovalov, O; Paulus, M; Sternemann, C; Toperverg, B P; Zabel, H

    2012-02-10

    We have investigated the structure and magnetism of self-assembled, 20 nm diameter iron oxide nanoparticles covered by an oleic acid shell for scrutinizing their structural and magnetic correlations. The nanoparticles were spin-coated on an Si substrate as a single monolayer and as a stack of 5 ML forming a multilayer. X-ray scattering (reflectivity and grazing incidence small-angle scattering) confirms high in-plane hexagonal correlation and a good layering property of the nanoparticles. Using polarized neutron reflectivity we have also determined the long range magnetic correlations parallel and perpendicular to the layers in addition to the structural ones. In a field of 5 kOe we determine a magnetization value of about 80% of the saturation value. At remanence the global magnetization is close to zero. However, polarized neutron reflectivity reveals the existence of regions in which magnetic moments of nanoparticles are well aligned, while losing order over longer distances. These findings confirm that in the nanoparticle assembly the magnetic dipole-dipole interaction is rather strong, dominating the collective magnetic properties at room temperature.

  16. Higher order structure analysis of nano-materials by spectral reflectance of laser-plasma soft x-ray

    International Nuclear Information System (INIS)

    Azuma, Hirozumi; Takeichi, Akihiro; Noda, Shoji

    1995-01-01

    We have proposed a new experimental arrangement to measure spectral reflectance of nano-materials for analyzing higher order structure with laser-plasma soft x-rays. Structure modification of annealed Mo/Si multilayers and a nylon-6/clay hybrid with poor periodicity was investigated. The measurement of the spectral reflectance of soft x-rays from laser-produced plasma was found to be a useful method for the structure analysis of nano-materials, especially those of rather poor periodicity

  17. X-ray reflectivity of cobalt and titanium in the vicinity of the Lsub(2,3) absorption edges

    International Nuclear Information System (INIS)

    Bremer, J.; Kaihola, L.; Keski-Kuha, R.

    1980-01-01

    X-ray reflectivity across cobalt and titanium Lsub(2,3) absorption edges was measured as a function of energy by means of continuous radiation from a tungsten anode in a grating spectrometer. The real and imaginary parts of the refractive index were obtained from the absorption curves and an exact Kramers-Kronig analysis. A measured fine structure in the reflected intensities was interpreted as an effect of white lines in the absorption spectra. The x-ray intensity was calculated as a function of energy by means of the Fresnel formula. (author)

  18. Integrated X-ray testing of the electro-optical breadboard model for the XMM reflection grating spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Bixler, J.V.; Craig, W.; Decker, T. [Lawrence Livermore National Lab., CA (United States); Aarts, H.; Boggende, T. den; Brinkman, A.C. [Space Research Organization Netherlands, Utrecht (Netherlands); Burkert, W.; Brauninger, H. [Max-Planck Institute fur Extraterrestische Physik, Testanlage (Germany); Branduardi-Raymont, G. [Univ. College London (United Kingdom); Dubbeldam, L. [Space Research Organization Netherlands, Leiden (Netherlands)] [and others

    1994-07-12

    X-ray calibration of the Electro-Optical Breadboard Model (EOBB) of the XXM Reflection Grating Spectrometer has been carried out at the Panter test facility in Germany. The EOBB prototype optics consisted of a four-shell grazing incidence mirror module followed by an array of eight reflection gratings. The dispersed x-rays were detected by an array of three CCDs. Line profile and efficiency measurements where made at several energies, orders, and geometric configurations for individual gratings and for the grating array as a whole. The x-ray measurements verified that the grating mounting method would meet the stringent tolerances necessary for the flight instrument. Post EOBB metrology of the individual gratings and their mountings confirmed the precision of the grating boxes fabrication. Examination of the individual grating surface`s at micron resolution revealed the cause of anomalously wide line profiles to be scattering due to the crazing of the replica`s surface.

  19. Testing the Kerr Black Hole Hypothesis Using X-Ray Reflection Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bambi, Cosimo; Nampalliwar, Sourabh [Center for Field Theory and Particle Physics and Department of Physics, Fudan University, 200433 Shanghai (China); Cárdenas-Avendaño, Alejandro [Programa de Matemática, Fundación Universitaria Konrad Lorenz, 110231 Bogotá (Colombia); Dauser, Thomas [Remeis Observatory and ECAP, Universität Erlangen-Nürnberg, D-96049 Bamberg (Germany); García, Javier A., E-mail: bambi@fudan.edu.cn [Harvard-Smithsonian Center for Astrophysics, Cambridge, MA 02138 (United States)

    2017-06-20

    We present the first X-ray reflection model for testing the assumption that the metric of astrophysical black holes is described by the Kerr solution. We employ the formalism of the transfer function proposed by Cunningham. The calculations of the reflection spectrum of a thin accretion disk are split into two parts: the calculation of the transfer function and the calculation of the local spectrum at any emission point in the disk. The transfer function only depends on the background metric and takes into account all the relativistic effects (gravitational redshift, Doppler boosting, and light bending). Our code computes the transfer function for a spacetime described by the Johannsen metric and can easily be extended to any stationary, axisymmetric, and asymptotically flat spacetime. Transfer functions and single line shapes in the Kerr metric are compared to those calculated from existing codes to check that we reach the necessary accuracy. We also simulate some observations with NuSTAR and LAD/eXTP and fit the data with our new model to show the potential capabilities of current and future observations to constrain possible deviations from the Kerr metric.

  20. Hydrogen concentration and mass density of diamondlike carbon films obtained by x-ray and neutron reflectivity

    DEFF Research Database (Denmark)

    Findeisen, E.; Feidenhans'l, R.; Vigild, Martin Etchells

    1994-01-01

    Specular reflectivity of neutrons and x rays can be used to determine the scattering length density profile of a material perpendicular to its surface. We have applied these techniques to study amorphous, diamondlike, hydrocarbon films. By the combination of these two techniques we obtain not onl...

  1. X-Ray Diffraction and Reflectivity Validation of the Depletion Attraction in the Competitive Adsorption of Lung Surfactant and Albumin

    DEFF Research Database (Denmark)

    Stenger, Patric C.; Wu, Guohui; Miller, Chad E.

    2009-01-01

    as on a pristine interface, but with a more compact lattice corresponding to a small increase in the surface pressure. These results confirm that albumin adsorption creates a physical barrier that inhibits LS adsorption, and that PEG in the subphase generates a depletion attraction between the LS aggregates...... to subsequent LS adsorption that can be overcome by the depletion attraction induced by polyethylene glycol (PEG) in solution. A combination of grazing incidence x-ray diffraction (GIXD), x-ray reflectivity (XR), and pressure-area isotherms provides molecular-resolution information on the location...

  2. X-ray absorption and reflection as probes of the GaN conduction bands: Theory and experiments

    Energy Technology Data Exchange (ETDEWEB)

    Lambrecht, W.R.L.; Rashkeev, S.N.; Segall, B. [Case Western Reserve Univ., Cleveland, OH (United States)] [and others

    1997-04-01

    X-ray absorption measurements are a well-known probe of the unoccupied states in a material. The same information can be obtained by using glancing angle X-ray reflectivity. In spite of several existing band structure calculations of the group III nitrides and previous optical studies in UV range, a direct probe of their conduction band densities of states is of interest. The authors performed a joint experimental and theoretical investigation using both of these experimental techniques for wurtzite GaN.

  3. Direct EUV/X-Ray Modulation of the Ionosphere During the August 2017 Total Solar Eclipse

    Science.gov (United States)

    Mrak, Sebastijan; Semeter, Joshua; Drob, Douglas; Huba, J. D.

    2018-05-01

    The great American total solar eclipse of 21 August 2017 offered a fortuitous opportunity to study the response of the atmosphere and ionosphere using a myriad of ground instruments. We have used the network of U.S. Global Positioning System receivers to examine perturbations in maps of ionospheric total electron content (TEC). Coherent large-scale variations in TEC have been interpreted by others as gravity wave-induced traveling ionospheric disturbances. However, the solar disk had two active regions at that time, one near the center of the disk and one at the edge, which resulted in an irregular illumination pattern in the extreme ultraviolet (EUV)/X-ray bands. Using detailed EUV occultation maps calculated from the National Aeronautics and Space Administration Solar Dynamics Observatory Atmospheric Imaging Assembly images, we show excellent agreement between TEC perturbations and computed gradients in EUV illumination. The results strongly suggest that prominent large-scale TEC disturbances were consequences of direct EUV modulation, rather than gravity wave-induced traveling ionospheric disturbances.

  4. High reflectance Cr/C multilayer at 250 eV for soft X-ray polarimetry

    Energy Technology Data Exchange (ETDEWEB)

    Wen, Mingwu; Jiang, Li; Zhang, Zhong; Huang, Qiushi [MOE Key Laboratory of Advanced Micro-Structured Materials, Institute of Precision Optical Engineering (IPOE), School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); Wang, Zhanshan, E-mail: wangzs@tongji.edu.cn [MOE Key Laboratory of Advanced Micro-Structured Materials, Institute of Precision Optical Engineering (IPOE), School of Physics Science and Engineering, Tongji University, Shanghai 200092 (China); She, Rui; Feng, Hua [Department of Engineering Physics, Tsinghua University, Beijing (China); Wang, Hongchang [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom)

    2015-10-01

    X-ray reflection near 45° via multilayer mirrors can be used for astronomical polarization measurements. A Cr/C multilayer mirror (designed for X-ray polarimetry at 250 eV), with a period thickness of 3.86 nm and a bi-layer number of 100, was fabricated using direct current magnetron sputtering. Grazing incidence X-ray reflectometry at 8 keV and transmission electron microscopy were used to investigate the multilayer structure. Different models were introduced to fit the hard X-ray reflectivity curve, which indicates that the layer thickness of two materials slightly drifts from the bottom to the top of the stack. Both the chromium and carbon layers are amorphous with asymmetric interfaces, while the Cr-on-C interface is slightly wider. Based on the good quality of the multilayer structure, a high reflectivity of 21.8% for the s-polarized light was obtained at 250 eV at a grazing incidence angle of 40.7°. The fabricated Cr/C multilayer mirror exhibits high reflectivity and polarization levels in the energy region of 240 eV–260 eV. - Highlights: • We fabricated Cr/C multilayer with 3.8 nm d-spacing. • X-ray reflectometry was used to determine the exact structure of Cr/C multilayer. • A high reflectivity of 21.8% for the s-polarized light was obtained at 250 eV. • Both Cr and C were found to be amorphous with slightly asymmetric interfaces. • A 4-layer model was used to fit and explain the results.

  5. X-ray Reflectivity Study of Ionic Liquids at Electrified Surfaces

    Science.gov (United States)

    Chu, Miaoqi

    X-ray reflectivity (XRR) versatile technique that characterize the surface structures. However, due to the lack of phase information of X-ray data, the reconstruction of electron density profile (EDP) from XRR data is an ill-posed inverse problem that requires extra attention. In Chapter 1, several key concepts in XRR data analysis are reviewed. The typical XRR data acquisition procedure and methods of modeling electron density are introduced. The widely used logarithm form of merit function is justified with mathematical deduction and numerical experiment. A scheme that generates artificial reflectivity data with theoretical statistical error but not systematical error is proposed. With the methods and schemes described in Chapter 1, simulated reflectivity data of a simple one-slab model is generated and fitted to test the efficient of EDP reconstruction. By isolating the parameters, the effects of slab width, electron density contrast and maximal wave transfer are studied individually. It?s demonstrated that best-fit/global minima, result reported by most XRR studies, don?t necessary reflect the real EDP. By contrast, mapping the merit function in the parametric space can capture much more details. Additionally, the widely accepted concept about the XRR theoretical spatial resolution (pi/q_{max}) as well the using Patterson function are brought to test. In the perspective of XRR data analysis, this chapter puts forward general rules to design and optimize XRR experiments. It also demonstrates how susceptible the fitting result will be if it?s not done carefully. In Chapter 3, the interface between hydrophobic OTS film and several solvents is studied with XRR in a transmission-cell setup. The solvents, from water, acetone, to alcohol (methanol, ethanol, 1-propanol), to alkane (pentane, hexane and heptane), vary significantly in terms of polarity and hydrogen bonding. However, the XRR data from different solvents are subtle. The methods and principles elicited in

  6. RefleX: X-ray absorption and reflection in active galactic nuclei for arbitrary geometries

    Science.gov (United States)

    Paltani, S.; Ricci, C.

    2017-11-01

    Reprocessed X-ray radiation carries important information about the structure and physical characteristics of the material surrounding the supermassive black hole (SMBH) in active galactic nuclei (AGN). We report here on a newly developed simulation platform, RefleX, which allows to reproduce absorption and reflection by quasi-arbitrary geometries. We show here the reliability of our approach by comparing the results of our simulations with existing spectral models such as pexrav, MYTorus and BNTorus. RefleX implements both Compton scattering on free electrons and Rayleigh scattering and Compton scattering on bound electrons. We show the effect of bound-electron corrections on a torus geometry simulated like in MYTorus. We release with this paper the RefleX executable, as well as RXTorus, a model that assumes absorption and reflection from a torus with a varying ratio of the minor to major axis of the torus. To allow major flexibility RXTorus is also distributed in three components: absorbed primary emission, scattered radiation and fluorescent lines. RXTorus is provided for different values of the abundance, and with (atomic configuration) or without (free-electron configuration) taking into account Rayleigh scattering and bound electrons. We apply the RXTorus model in both configurations on the XMM-Newton and NuSTAR spectrum of the Compton-thick AGN NGC 424 and find that the models are able to reproduce very well the observations, but that the assumption on the bound or free state of the electrons has significant consequences on the fit parameters. RefleX executable, user manual and example models are available at http://www.astro.unige.ch/reflex. A copy of the RefleX executable is also available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/607/A31

  7. Total porosity of carbonate reservoir rocks by X-ray microtomography in two different spatial resolutions

    International Nuclear Information System (INIS)

    Nagata, Rodrigo; Appoloni, Carlos R.; Marques, Leonardo C.; Fernandes, Celso P.

    2011-01-01

    Carbonate reservoir rocks contain more than 50% of world's petroleum. To know carbonate rocks' structural properties is quite important to petroleum extraction. One of their main structural properties is the total porosity, which shows the rock's capacity to stock petroleum. In recent years, the X-ray microtomography had been used to analyze the structural parameters of reservoir rocks. Such nondestructive technique generates images of the samples' internal structure, allowing the evaluation of its properties. The spatial resolution is a measurement parameter that indicates the smallest structure size observable in a sample. It is possible to measure one sample using two or more different spatial resolutions in order to evaluate the samples' pore scale. In this work, two samples of the same sort of carbonate rock were measured, and in each measurement a different spatial resolution (17 μm and 7 μm) was applied. The obtained results showed that with the better resolution it was possible to measure 8% more pores than with the poorer resolution. Such difference provides us with good expectations about such approach to study the pore scale of carbonate rocks. (author)

  8. Visualization of femorotibial contact in total knee arthroplasty using X-ray fluoroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yamazaki, Takaharu E-mail: yamazaki@image.med.osaka-u.ac.jp; Watanabe, Tetsu; Nakajima, Yoshikazu; Sugamoto, Kazuomi; Tomita, Tetsuya; Maeda, Daisuke; Sahara, Wataru; Yoshikawa, Hideki; Tamura, Shinichi

    2005-01-01

    The purpose of this study was to build a visualization technique of the femorotibial contact in fixed-bearing total knee arthroplasty (TKA) using X-ray fluoroscopy, and to apply this technique to a TKA patient during dynamic motion. In vivo kinametcis of the metallic knee implant was determined using a 2D/3D registration technique, which uses computer assisted design (CAD) model of the implant to estimate the 3D pose of radiopaque metallic femoral and tibial components from a single-plane fluoroscopic image. In fixed-bearing TKA, a 3D pose of radiolucent tibial polyethylene insert can be determined from the estimated pose of the tibial component. To visualize femorotibial contact, the proximity between surfaces of femoral component and tibial insert was calculated, and mapped onto the insert surface model. For the clinical application, dynamic states of contact on the tibial insert were observed including axial rotation and unilateral loading during knee flexion, and post-cam contact of posterior stabilized TKA. The present technique provided us new information and enabled us to better understand the relationship between in vivo knee kinematics and articular shape of the implant.

  9. X-ray fluorescence imaging with polycapillary X-ray optics

    International Nuclear Information System (INIS)

    Yonehara, Tasuku; Yamaguchi, Makoto; Tsuji, Kouichi

    2010-01-01

    X-ray fluorescence spectrometry imaging is a powerful tool to provide information about the chemical composition and elemental distribution of a specimen. X-ray fluorescence spectrometry images were conventionally obtained by using a μ-X-ray fluorescence spectrometry spectrometer, which requires scanning a sample. Faster X-ray fluorescence spectrometry imaging would be achieved by eliminating the process of sample scanning. Thus, we developed an X-ray fluorescence spectrometry imaging instrument without sample scanning by using polycapillary X-ray optics, which had energy filter characteristics caused by the energy dependence of the total reflection phenomenon. In the present paper, we show that two independent straight polycapillary X-ray optics could be used as an energy filter of X-rays for X-ray fluorescence. Only low energy X-rays were detected when the angle between the two optical axes was increased slightly. Energy-selective X-ray fluorescence spectrometry images with projection mode were taken by using an X-ray CCD camera equipped with two polycapillary optics. It was shown that Fe Kα (6.40 keV) and Cu Kα (8.04 keV) could be discriminated for Fe and Cu foils.

  10. The feasibility of 10 keV X-ray as radiation source in total dose response radiation test

    International Nuclear Information System (INIS)

    Li Ruoyu; Li Bin; Luo Hongwei; Shi Qian

    2005-01-01

    The standard radiation source utilized in traditional total dose response radiation test is 60 Co, which is environment-threatening. X-rays, as a new radiation source, has the advantages such as safety, precise control of dose rate, strong intensity, possibility of wafer-level test or even on-line test, which greatly reduce cost for package, test and transportation. This paper discussed the feasibility of X-rays replacing 60 Co as the radiation source, based on the radiation mechanism and the effects of radiation on gate oxide. (authors)

  11. Single-Residue Sensitivity in Neutron Reflectivity and Resonant X-ray Reflectivity from Langmuir Monolayers of Synthetic Peptides

    Science.gov (United States)

    Strzalka, Joseph; Satija, Sushil; Dimasi, Elaine; Kuzmenko, Ivan; Gog, Thomas; Blasie, J. Kent

    2004-03-01

    Labeling groups with ^2H to distinguish them in the scattering length density (SLD) profile constitutes the chief advantage of neutron reflectivity (NR) in studying Langmuir monolayers (LM) of lipids and proteins. Solid phase synthesis (SPPS) permits the labeling of a single residue in a peptide. Recent work demonstrates the sensitivity of NR to single ^2H-labeled residues in LM of vectorially oriented α -helical bundle peptides. NR requires comparison of isomorphic samples of all-^1H and ^2H-labeled peptides. Alternately, resonant x-ray reflectivity (RXR) uses only one sample. RXR exploits energy-dependent changes in the scattering factor from heavy atoms to distinguish them within the SLD profile. Peptides may be labeled by SPPS (e.g. Br-Phe), or may have inherent labels (e.g. Fe in heme proteins). As test cases, we studied LM of Br-labeled lipids and peptides with RXR. Both approaches require a model-independent means of obtaining SLD profiles from the reflectivity data. We have applied box-refinement to obtain the gradient SLD profile. This is fit uniquely with a sum of Gaussians and integrated analytically [Blasie et al., PRB 67 224201 (2003)] to provide the SLD profile. Label positions can then be determined to sub-Ångstrom accuracy. This work supported by the NIH (GM55876).

  12. Evaluation of the soft x-ray reflectivity of micropore optics using anisotropic wet etching of silicon wafers.

    Science.gov (United States)

    Mitsuishi, Ikuyuki; Ezoe, Yuichiro; Koshiishi, Masaki; Mita, Makoto; Maeda, Yoshitomo; Yamasaki, Noriko Y; Mitsuda, Kazuhisa; Shirata, Takayuki; Hayashi, Takayuki; Takano, Takayuki; Maeda, Ryutaro

    2010-02-20

    The x-ray reflectivity of an ultralightweight and low-cost x-ray optic using anisotropic wet etching of Si (110) wafers is evaluated at two energies, C K(alpha)0.28 keV and Al K(alpha)1.49 keV. The obtained reflectivities at both energies are not represented by a simple planar mirror model considering surface roughness. Hence, an geometrical occultation effect due to step structures upon the etched mirror surface is taken into account. Then, the reflectivities are represented by the theoretical model. The estimated surface roughness at C K(alpha) (approximately 6 nm rms) is significantly larger than approximately 1 nm at Al K(alpha). This can be explained by different coherent lengths at two energies.

  13. Evaluation of the soft x-ray reflectivity of micropore optics using anisotropic wet etching of silicon wafers

    Energy Technology Data Exchange (ETDEWEB)

    Mitsuishi, Ikuyuki; Ezoe, Yuichiro; Koshiishi, Masaki; Mita, Makoto; Maeda, Yoshitomo; Yamasaki, Noriko Y.; Mitsuda, Kazuhisa; Shirata, Takayuki; Hayashi, Takayuki; Takano, Takayuki; Maeda, Ryutaro

    2010-02-20

    The x-ray reflectivity of an ultralightweight and low-cost x-ray optic using anisotropic wet etching of Si (110) wafers is evaluated at two energies, C K{alpha}0.28 keV and Al K{alpha}1.49 keV. The obtained reflectivities at both energies are not represented by a simple planar mirror model considering surface roughness. Hence, an geometrical occultation effect due to step structures upon the etched mirror surface is taken into account. Then, the reflectivities are represented by the theoretical model. The estimated surface roughness at C K{alpha} ({approx}6 nm rms) is significantly larger than {approx}1 nm at Al K{alpha}. This can be explained by different coherent lengths at two energies.

  14. Reflections on hard X-ray photon-in/photon-out spectroscopy for electronic structure studies

    Energy Technology Data Exchange (ETDEWEB)

    Glatzel, Pieter, E-mail: glatzel@esrf.fr [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Weng, Tsu-Chien; Kvashnina, Kristina; Swarbrick, Janine; Sikora, Marcin [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Gallo, Erik [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Department of Inorganic, Physical and Materials Chemistry, INSTM Reference Center and NIS Centre of Excellence, Università di Torino, Via P. Giuria 7, I-10125 Torino (Italy); Smolentsev, Nikolay [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Research Center for Nanoscale Structure of Matter, Southern Federal University, str. Zorge 5, 344090 Rostov-on-Don (Russian Federation); Mori, Roberto Alonso [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France)

    2013-06-15

    Highlights: ► Overview of some recent developments in hard X-ray RXES/RIXS. ► Evaluation of spectral line broadening in RXES/RIXS. ► Modelling of RXES/RIXS by ground state DFT calculations. ► Discussion on when HERFD provides a good approximation to XAS. -- Abstract: An increasing community of researchers in various fields of natural sciences is combining X-ray absorption with X-ray emission spectroscopy (XAS–XES) to study electronic structure. With the applications becoming more diverse, the objectives and the requirements in photon-in/photon-out spectroscopy are becoming broader. It is desirable to find simple experimental protocols, robust data reduction and theoretical tools that help the experimentalist to understand their data and learn about the electronic structure. This article presents a collection of considerations on non-resonant and resonant XES with the aim to guide the experimentalist to make good use of this technique.

  15. Reflectivity around the gold L-edges of X-ray reector of the soft X-ray telescope onboard ASTRO-H

    DEFF Research Database (Denmark)

    Maeda, Yoshitomo; Kikuchi, Naomichi; Kurashima, Sho

    2017-01-01

    We report the atomic scattering factor in the 11.2-15.4 keV for the ASTRO-H Soft X-ray Telescope (SXT)9 obtained in the ground based measurements. The large effective area of the SXT covers above 10 keV. In fact, the flight data show the spectra of the celestical objects in the hard X-ray band. I...

  16. Diffuse X-ray scattering near the Bragg reflection of P-doped Czochralski silicon

    International Nuclear Information System (INIS)

    Stojanoff, V.; Pimentel, C.A.F.

    1983-01-01

    Bragg line profile and high resolution diffuse X-ray scattering measurements around the (400) reciprocal lattice point of dislocation-free Czochralski Si single crystals P-doped have shown defects of interstitial nature with typical size about 1000 A. (Author) [pt

  17. Energy-dispersive X-ray reflectivity and GID for real-time growth studies of pentacene thin films

    International Nuclear Information System (INIS)

    Kowarik, S.; Gerlach, A.; Leitenberger, W.; Hu, J.; Witte, G.; Woell, C.; Pietsch, U.; Schreiber, F.

    2007-01-01

    We use energy-dispersive X-ray reflectivity and grazing incidence diffraction (GID) to follow the growth of the crystalline organic semiconductor pentacene on silicon oxide in-situ and in real-time. The technique allows for monitoring Bragg reflections and measuring X-ray growth oscillations with a time resolution of 1 min in a wide q-range in reciprocal space extending over 0.25-0.80 A -1 , i.e. sampling a large number of Fourier components simultaneously. A quantitative analysis of growth oscillations at several q-points yields the evolution of the surface roughness, showing a marked transition from layer-by-layer growth to strong roughening after four monolayers of pentacene have been deposited

  18. Errors in the determination of the total filtration of diagnostic x-ray tubes by the HVL method

    International Nuclear Information System (INIS)

    Gilmore, B.J.; Cranley, K.

    1990-01-01

    Optimal technique and an analysis of errors are essential for interpreting whether the total filtration of a diagnostic x-ray tube is acceptable. The study discusses this problem from a theoretical viewpoint utilising recent theoretical HVL-total-filtration data relating to 10 0 and 16 0 tungsten target angles and 0-30% kilovoltage ripples. The theory indicates the typical accuracy to which each appropriate parameter must be determined to maintain acceptable errors in total filtration. A quantitative approach is taken to evaluate systematic errors in a technique for interpolation of HVL from raw attenuation curve data. A theoretical derivation is presented to enable random errors in HVL due to x-ray set inconsistency to be estimated for particular experimental techniques and data analysis procedures. Further formulae are presented to enable errors in the total filtration estimate to be readily determined from those in the individual parameters. (author)

  19. CRL X-ray tube

    International Nuclear Information System (INIS)

    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. (authors)

  20. Dual X-ray absortiometry(DXA) in the detection of loosening in the total hip replacement arthroplasty: preliminary study

    International Nuclear Information System (INIS)

    Yoon, Hye Kyung; Kang, Heung Sik; Han, Man Chung; Kim, Hee Joong; Kim, Young Min

    1994-01-01

    Algorithms to get cross-sectional bone density pattern(transverse histogram) to predict the loosening of hip prosthesis using DXA(Dual X-ray Absorptiometry) have been developed. We performed this study to analyze the correlation between radiologic findings and densitometric pattern of the THRA(Total Hip Replacement Arthroplasty) patients. Thirty-six hips of 32 THRA patients were evaluated. The duration between THRA and DXA was from 1 year 7 months to 15 years. On transverse histogram, the periprosthetic bone density patterns were classified as 3 types; type I , rigid fixation in 17, type II definite loosening in 8, and type III, partial loosening in 11 cases. Surgical findings, plain X-ray findings and transverse histogram using DXA were correlated. Among 14 cases performing revision for acetabular prosthesis loosening, 5 cases revealed loosening of femoral stems while 9 cases revealed rigid fixation of femoral stems. Sensitivity was 100% for either plain X-ray or DXA. Specificity was 88%, 77% for plain X-ray and DXA respectively. This preliminary study reveals that periprosthetic bone density pattern on transverse histogram on DXA may be useful in the evaluation of the loosening. However, further study will be needed for clinical application

  1. A high-density relativistic reflection origin for the soft and hard X-ray excess emission from Mrk 1044

    Science.gov (United States)

    Mallick, L.; Alston, W. N.; Parker, M. L.; Fabian, A. C.; Pinto, C.; Dewangan, G. C.; Markowitz, A.; Gandhi, P.; Kembhavi, A. K.; Misra, R.

    2018-06-01

    We present the first results from a detailed spectral-timing analysis of a long (˜130 ks) XMM-Newton observation and quasi-simultaneous NuSTAR and Swift observations of the highly-accreting narrow-line Seyfert 1 galaxy Mrk 1044. The broadband (0.3-50 keV) spectrum reveals the presence of a strong soft X-ray excess emission below ˜1.5 keV, iron Kα emission complex at ˜6 -7 keV and a `Compton hump' at ˜15 -30 keV. We find that the relativistic reflection from a high-density accretion disc with a broken power-law emissivity profile can simultaneously explain the soft X-ray excess, highly ionized broad iron line and the Compton hump. At low frequencies ([2 - 6] × 10-5 Hz), the power-law continuum dominated 1.5-5 keV band lags behind the reflection dominated 0.3-1 keV band, which is explained with a combination of propagation fluctuation and Comptonization processes, while at higher frequencies ([1 - 2] × 10-4 Hz), we detect a soft lag which is interpreted as a signature of X-ray reverberation from the accretion disc. The fractional root-mean-squared (rms) variability of the source decreases with energy and is well described by two variable components: a less variable relativistic disc reflection and a more variable direct coronal emission. Our combined spectral-timing analyses suggest that the observed broadband X-ray variability of Mrk 1044 is mainly driven by variations in the location or geometry of the optically thin, hot corona.

  2. X-RAY REFLECTED SPECTRA FROM ACCRETION DISK MODELS. I. CONSTANT DENSITY ATMOSPHERES

    International Nuclear Information System (INIS)

    Garcia, J.; Kallman, T. R.

    2010-01-01

    We present new models for illuminated accretion disks, their structure, and reprocessed emission. We consider the effects of incident X-rays on the surface of an accretion disk by simultaneously solving the equations of radiative transfer, energy balance, and ionization equilibrium over a large range of column densities. We assume plane-parallel geometry and azimuthal symmetry, such that each calculation corresponds to a ring at a given distance from the central object. Our models include recent and complete atomic data for K-shell processes of the iron and oxygen isonuclear sequences. We examine the effect on the spectrum of fluorescent Kα line emission and absorption in the emitted spectrum. We also explore the dependence of the spectrum on the strength of the incident X-rays and other input parameters, and discuss the importance of Comptonization on the emitted spectrum.

  3. Measurement of total calcium in neurons by electron probe X-ray microanalysis.

    Science.gov (United States)

    Pivovarova, Natalia B; Andrews, S Brian

    2013-11-20

    In this article the tools, techniques, and instruments appropriate for quantitative measurements of intracellular elemental content using the technique known as electron probe microanalysis (EPMA) are described. Intramitochondrial calcium is a particular focus because of the critical role that mitochondrial calcium overload plays in neurodegenerative diseases. The method is based on the analysis of X-rays generated in an electron microscope (EM) by interaction of an electron beam with the specimen. In order to maintain the native distribution of diffusible elements in electron microscopy specimens, EPMA requires "cryofixation" of tissue followed by the preparation of ultrathin cryosections. Rapid freezing of cultured cells or organotypic slice cultures is carried out by plunge freezing in liquid ethane or by slam freezing against a cold metal block, respectively. Cryosections nominally 80 nm thick are cut dry with a diamond knife at ca. -160 °C, mounted on carbon/pioloform-coated copper grids, and cryotransferred into a cryo-EM using a specialized cryospecimen holder. After visual survey and location mapping at ≤-160 °C and low electron dose, frozen-hydrated cryosections are freeze-dried at -100 °C for ~30 min. Organelle-level images of dried cryosections are recorded, also at low dose, by means of a slow-scan CCD camera and subcellular regions of interest selected for analysis. X-rays emitted from ROIs by a stationary, focused, high-intensity electron probe are collected by an energy-dispersive X-ray (EDX) spectrometer, processed by associated electronics, and presented as an X-ray spectrum, that is, a plot of X-ray intensity vs. energy. Additional software facilitates: 1) identification of elemental components by their "characteristic" peak energies and fingerprint; and 2) quantitative analysis by extraction of peak areas/background. This paper concludes with two examples that illustrate typical EPMA applications, one in which mitochondrial calcium analysis

  4. Design of a bolometer for total-energy measurement of the linear coherent light source pulsed X-ray laser

    International Nuclear Information System (INIS)

    Friedrich, S.; Li, L.; Ott, L.L.; Kolgani, Rajeswari M.; Yong, G.J.; Ali, Z.A.; Drury, O.B.; Ables, E.; Bionta, R.M.

    2006-01-01

    We are developing a cryogenic bolometer to measure the total energy of the linear coherent light source (LCLS) free electron X-ray laser to be built at the Stanford Linear Accelerator Center. The laser will produce ultrabright X-ray pulses in the energy range between 0.8 and 8 keV with ∼10 12 photons per ∼200 fs pulse at a repeat interval of 8 ms, and will be accompanied by a halo of spontaneous undulator radiation. The bolometer is designed to determine the total energy of each laser pulse to within (1- x ) Sr x MnO 3 sensor array at the metal-insulator transition, where the composition x is adjusted to produce the desired transition temperature. We discuss design considerations and material choices, and present numerical simulations of the thermal response

  5. Analysis of x-ray reflectivity data from low-contrast polymer bilayer systems using a Fourier method

    International Nuclear Information System (INIS)

    Seeck, O. H.; Kaendler, I. D.; Tolan, M.; Shin, K.; Rafailovich, M. H.; Sokolov, J.; Kolb, R.

    2000-01-01

    X-ray reflectivity data of polymer bilayer systems have been analyzed using a Fourier method which takes into account different limits of integration in q-space. It is demonstrated that the interfacial parameters can be determined with high accuracy although the difference in the electron density (the contrast) of the two polymers is extremely small. This method is not restricted to soft-matter thin films. It can be applied to any reflectivity data from low-contrast layer systems. (c) 2000 American Institute of Physics

  6. NUSTAR and Suzaku x-ray spectroscopy of NGC 4151: Evidence for reflection from the inner accretion disk

    Energy Technology Data Exchange (ETDEWEB)

    Keck, M. L.; Brenneman, L. W.; Ballantyne, D. R.; Bauer, F.; Boggs, S. E.; Christensen, F. E.; Craig, W. W.; Dauser, T.; Elvis, M.; Fabian, A. C.; Fuerst, F.; García, J.; Grefenstette, B. W.; Hailey, C. J.; Harrison, F. A.; Madejski, G.; Marinucci, A.; Matt, G.; Reynolds, C. S.; Stern, D.; Walton, D. J.; Zoghbi, A.

    2015-06-15

    We present X-ray timing and spectral analyses of simultaneous 150 ks Nuclear Spectroscopic Telescope Array (NuSTAR) and Suzaku X-ray observations of the Seyfert 1.5 galaxy NGC 4151. We disentangle the continuum emission, absorption, and reflection properties of the active galactic nucleus (AGN) by applying inner accretion disk reflection and absorption-dominated models. With a time-averaged spectral analysis, we find strong evidence for relativistic reflection from the inner accretion disk. We find that relativistic emission arises from a highly ionized inner accretion disk with a steep emissivity profile, which suggests an intense, compact illuminating source. We find a preliminary, near-maximal black hole spin $a\\gt 0.9$ accounting for statistical and systematic modeling errors. We find a relatively moderate reflection fraction with respect to predictions for the lamp post geometry, in which the illuminating corona is modeled as a point source. Through a time-resolved spectral analysis, we find that modest coronal and inner disk reflection (IDR) flux variation drives the spectral variability during the observations. We discuss various physical scenarios for the IDR model and we find that a compact corona is consistent with the observed features.

  7. The X-Ray Reflection Spectrum of the Radio-Loud Quasar 4C 74.26

    Science.gov (United States)

    Lohfink, Ann M.; Fabian, Andrew C.; Ballantyne, David R.; Boggs, S. E.; Boorman, Peter; Christensen, F. E.; Craig, W. W.; Farrah, Duncan; Garcia, Javier; Hailey, C. J.; hide

    2017-01-01

    The relativistic jets created by some active galactic nuclei are important agents of AGN feedback. In spite of this, our understanding of what produces these jets is still incomplete. X-ray observations, which can probe the processes operating in the central regions in the immediate vicinity of the supermassive black hole, the presumed jet launching point, are potentially particularly valuable in illuminating the jet formation process. Here, we present the hard X-ray NuSTAR observations of the radio-loud quasar 4C 74.26 in a joint analysis with quasi-simultaneous, soft X-ray Swift observations. Our spectral analysis reveals a high-energy cutoff of -183+3551 keV and confirms the presence of ionized reflection in the source. From the average spectrum we detect that the accretion disk is mildly recessed, with an inner radius of Rin4180 Rg. However, no significant evolution of the inner radius is seen during the three months covered by our NuSTAR campaign. This lack of variation could mean that the jet formation in this radio-loud quasar differs from what is observed in broad-line radio galaxies.

  8. Restoring efficiency of hemopoietic cell transplantation in a mouse lethally irradiated by a total exposure to X rays

    International Nuclear Information System (INIS)

    Doria, Gino

    1959-10-01

    This research thesis reports the study of possibility of treatments (or restoration) of a mouse which has been submitted to a lethal dose of X rays. More particularly, the author compared the restoring efficiency of bone marrow and fetal liver injected in a mouse which had been lethally irradiated by a total exposure to X rays. He also studied the functional status of the hemopoietic graft, and the emergence of the secondary disease in mice which had been as well lethally irradiated and then restored by injection of bone marrow and fetal liver. The author then addressed the influence of the induction of immune tolerance of the host with respect to the donor on the survival of a mouse lethally irradiated and restored by homologue bone marrow [fr

  9. Insight into the structure of Pd/ZrO2 during the total oxidation of methane using combined in situ XRD, X.-ray absorption and Raman spectroscopy

    DEFF Research Database (Denmark)

    Grunwaldt, Jan-Dierk; van Vegten, Niels; Baiker, Alfons

    2009-01-01

    The structure of palladium during the total combustion of methane has been studied by a combination of the complementary in situ techniques X-ray absorption spectroscopy, Raman spectroscopy and X-ray diffraction. The study demonstrates that finely dispersed and oxidized palladium is most active f...

  10. Determination of wafer bonding mechanisms for plasma activated SiN films with x-ray reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Hayashi, S [Department of Materials Science and Engineering, University of California, Los Angeles, CA 90095 (United States); Sandhu, R [Department of Materials Science and Engineering, University of California, Los Angeles, CA 90095 (United States); Wojtowicz, M [Northrop Grumman Space Technology, Redondo Beach, CA 90278 (United States); Sun, Y [Department of Chemical Engineering, University of California, Los Angeles, CA 90095 (United States); Hicks, R [Department of Chemical Engineering, University of California, Los Angeles, CA 90095 (United States); Goorsky, M S [Department of Materials Science and Engineering, University of California, Los Angeles, CA 90095 (United States)

    2005-05-21

    Specular and diffuse x-ray reflectivity measurements were employed for wafer bonding studies of surface and interfacial reactions in {approx}800 A thick SiN films deposited on III-V substrates. CuK{sub {alpha}}{sub 1} radiation was employed for these measurements. The as-deposited films show very low surface roughness and uniform, high density SiN. Reflectivity measurements show that an oxygen plasma treatment converts the nitride surface to a somewhat porous SiO{sub x} layer (67 A thick, at 80% of SiO{sub 2} density), with confirmation of the oxide formation from x-ray photoelectron spectroscopy. Reactions at the bonded interface of two oxygen plasma treated SiN layers were examined using a bonded structure from which one of the III-V wafers is removed. Reflectivity measurements of bonded structures annealed at 150 deg. C and 300 deg. C show an increase in the SiO{sub x} layer density and thickness and even a density gradient across this interface. The increase in density is correlated with an increase in bond strength, where after the 300 deg. C anneal, a high interfacial bond strength, exceeding the bulk strength, was achieved.

  11. Center for X-Ray Optics, 1992

    International Nuclear Information System (INIS)

    1993-08-01

    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

  12. Fullerene films and fullerene-dodecylamine adduct monolayers at air-water interfaces studied by neutron and x-ray reflection

    DEFF Research Database (Denmark)

    Wang, J.Y.; Vaknin, D.; Uphaus, R.A.

    1994-01-01

    Neutron and X-ray reflection measurements and surface pressure isotherms of spread films of the fullerene-dodecylamine adduct C60-[NH2(CH2)11CH3]x all indicate that this material may form monomolecular layers on water surfaces. The reflection data sets (neutron on both H2O and D2O) can be accounted...... for by a single model structure defined in terms of the dimensions of an average cell and its chemical composition. This model ascribes a total thickness of about 29 angstrom to the molecular interface layer with the following internal structure. The fullerenes (with several alkyl chains attached) form a central...... stratum and the remainder alkyl tails are located close to both the air and the water interfaces. The alkyl moieties close to the aqueous substrate are hydrated. The reflection experiments and the isotherms suggest that on average 8 +/- 3 dodecylamine molecules are present per fullerene, consistent within...

  13. Quantitative resonant soft x-ray reflectivity of ultrathin anisotropic organic layers: Simulation and experiment of PTCDA on Au

    International Nuclear Information System (INIS)

    Capelli, R.; Koshmak, K.; Giglia, A.; Mukherjee, S.; Nannarone, S.; Mahne, N.; Doyle, B. P.; Pasquali, L.

    2016-01-01

    Resonant soft X-ray reflectivity at the carbon K edge, with linearly polarized light, was used to derive quantitative information of film morphology, molecular arrangement, and electronic orbital anisotropies of an ultrathin 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) film on Au(111). The experimental spectra were simulated by computing the propagation of the electromagnetic field in a trilayer system (vacuum/PTCDA/Au), where the organic film was treated as an anisotropic medium. Optical constants were derived from the calculated (through density functional theory) absorption cross sections of the single molecule along the three principal molecular axes. These were used to construct the dielectric tensor of the film, assuming the molecules to be lying flat with respect to the substrate and with a herringbone arrangement parallel to the substrate plane. Resonant soft X-ray reflectivity proved to be extremely sensitive to film thickness, down to the single molecular layer. The best agreement between simulation and experiment was found for a film of 1.6 nm, with flat laying configuration of the molecules. The high sensitivity to experimental geometries in terms of beam incidence and light polarization was also clarified through simulations. The optical anisotropies of the organic film were experimentally determined and through the comparison with calculations, it was possible to relate them to the orbital symmetry of the empty electronic states.

  14. Quantitative resonant soft x-ray reflectivity of ultrathin anisotropic organic layers: Simulation and experiment of PTCDA on Au

    Energy Technology Data Exchange (ETDEWEB)

    Capelli, R.; Koshmak, K.; Giglia, A.; Mukherjee, S.; Nannarone, S. [IOM-CNR, s.s. 14, Km. 163.5 in AREA Science Park, Basovizza, 34149 Trieste (Italy); Mahne, N. [Elettra, s.s. 14, km 163.5 in AREA Science Park, Basovizza, 34149 Trieste (Italy); Doyle, B. P. [Department of Physics, University of Johannesburg, P.O. Box 524, Auckland Park 2006 (South Africa); Pasquali, L., E-mail: luca.pasquali@unimore.it [IOM-CNR, s.s. 14, Km. 163.5 in AREA Science Park, Basovizza, 34149 Trieste (Italy); Department of Physics, University of Johannesburg, P.O. Box 524, Auckland Park 2006 (South Africa); Dipartimento di Ingegneria “Enzo Ferrari,” Università di Modena e Reggio Emilia, Via Vignolese 905, 41125 Modena (Italy)

    2016-07-14

    Resonant soft X-ray reflectivity at the carbon K edge, with linearly polarized light, was used to derive quantitative information of film morphology, molecular arrangement, and electronic orbital anisotropies of an ultrathin 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) film on Au(111). The experimental spectra were simulated by computing the propagation of the electromagnetic field in a trilayer system (vacuum/PTCDA/Au), where the organic film was treated as an anisotropic medium. Optical constants were derived from the calculated (through density functional theory) absorption cross sections of the single molecule along the three principal molecular axes. These were used to construct the dielectric tensor of the film, assuming the molecules to be lying flat with respect to the substrate and with a herringbone arrangement parallel to the substrate plane. Resonant soft X-ray reflectivity proved to be extremely sensitive to film thickness, down to the single molecular layer. The best agreement between simulation and experiment was found for a film of 1.6 nm, with flat laying configuration of the molecules. The high sensitivity to experimental geometries in terms of beam incidence and light polarization was also clarified through simulations. The optical anisotropies of the organic film were experimentally determined and through the comparison with calculations, it was possible to relate them to the orbital symmetry of the empty electronic states.

  15. Background estimation in short-wave region during determination of total sample composition by x-ray fluorescence method

    International Nuclear Information System (INIS)

    Simakov, V.A.; Kordyukov, S.V.; Petrov, E.N.

    1988-01-01

    Method of background estimation in short-wave spectral region during determination of total sample composition by X-ray fluorescence method is described. 13 types of different rocks with considerable variations of base composition and Zr, Nb, Th, U content below 7x10 -3 % are investigated. The suggested method of background accounting provides for a less statistical error of the background estimation than direct isolated measurement and reliability of its determination in a short-wave region independent on the sample base. Possibilities of suggested method for artificial mixtures conforming by the content of main component to technological concemtrates - niobium, zirconium, tantalum are estimated

  16. Detection of Reflection Features in the Neutron Star Low-mass X-Ray Binary Serpens X-1 with NICER

    Science.gov (United States)

    Ludlam, R. M.; Miller, J. M.; Arzoumanian, Z.; Bult, P. M.; Cackett, E. M.; Chakrabarty, D.; Enoto, T.; Fabian, A. C.; Gendreau, K. C.; Guillot, S.; Homan, J.; Jaisawal, G. K.; Keek, L.; La Marr, B.; Malacaria, C.; Markwardt, C. B.; Steiner, J. F.; Strohmayer, T. E.

    2018-05-01

    We present Neutron Star Interior Composition Explorer (NICER) observations of the neutron star (NS) low-mass X-ray binary Serpens X-1 during the early mission phase in 2017. With the high spectral sensitivity and low-energy X-ray passband of NICER, we are able to detect the Fe L line complex in addition to the signature broad, asymmetric Fe K line. We confirm the presence of these lines by comparing the NICER data to archival observations with XMM-Newton/Reflection Grating Spectrometer (RGS) and NuSTAR. Both features originate close to the innermost stable circular orbit (ISCO). When modeling the lines with the relativistic line model RELLINE, we find that the Fe L blend requires an inner disk radius of {1.4}-0.1+0.2 R ISCO and Fe K is at {1.03}-0.03+0.13 R ISCO (errors quoted at 90%). This corresponds to a position of {17.3}-1.2+2.5 km and {12.7}-0.4+1.6 km for a canonical NS mass ({M}NS}=1.4 {M}ȯ ) and dimensionless spin value of a = 0. Additionally, we employ a new version of the RELXILL model tailored for NSs and determine that these features arise from a dense disk and supersolar Fe abundance.

  17. Development and production of a multilayer-coated x-ray reflecting stack for the Athena mission

    Science.gov (United States)

    Massahi, S.; Ferreira, D. D. M.; Christensen, F. E.; Shortt, B.; Girou, D. A.; Collon, M.; Landgraf, B.; Barriere, N.; Krumrey, M.; Cibik, L.; Schreiber, S.

    2016-07-01

    The Advanced Telescope for High-Energy Astrophysics, Athena, selected as the European Space Agency's second large-mission, is based on the novel Silicon Pore Optics X-ray mirror technology. DTU Space has been working for several years on the development of multilayer coatings on the Silicon Pore Optics in an effort to optimize the throughput of the Athena optics. A linearly graded Ir/B4C multilayer has been deposited on the mirrors, via the direct current magnetron sputtering technique, at DTU Space. This specific multilayer, has through simulations, been demonstrated to produce the highest reflectivity at 6 keV, which is a goal for the scientific objectives of the mission. A critical aspect of the coating process concerns the use of photolithography techniques upon which we will present the most recent developments in particular related to the cleanliness of the plates. Experiments regarding the lift-off and stacking of the mirrors have been performed and the results obtained will be presented. Furthermore, characterization of the deposited thin-films was performed with X-ray reflectometry at DTU Space and in the laboratory of the Physikalisch-Technische Bundesanstalt at the synchrotron radiation facility BESSY II.

  18. Design of a bolometer for total-energy measurement of the linear coherent light source pulsed X-ray laser

    Energy Technology Data Exchange (ETDEWEB)

    Friedrich, S. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States)]. E-mail: Friedrich1@llnl.gov; Li, L. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States); Ott, L.L. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States); Kolgani, Rajeswari M. [Department of Physics, Geosciences and Astronomy, Towson University, 8000 York Avenue, Towson MD 21252 (United States); Yong, G.J. [Department of Physics, Geosciences and Astronomy, Towson University, 8000 York Avenue, Towson MD 21252 (United States); Ali, Z.A. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States); Drury, O.B. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States); Ables, E. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States); Bionta, R.M. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore CA 94550 (United States)

    2006-04-15

    We are developing a cryogenic bolometer to measure the total energy of the linear coherent light source (LCLS) free electron X-ray laser to be built at the Stanford Linear Accelerator Center. The laser will produce ultrabright X-ray pulses in the energy range between 0.8 and 8 keV with {approx}10{sup 12} photons per {approx}200 fs pulse at a repeat interval of 8 ms, and will be accompanied by a halo of spontaneous undulator radiation. The bolometer is designed to determine the total energy of each laser pulse to within <0.1%, taking into account thermal and mechanical stress to prevent melting in the LCLS beam due to its high energy density. We propose to use a magnetoresistive Nd{sub (1-} {sub x} {sub )}Sr {sub x} MnO{sub 3} sensor array at the metal-insulator transition, where the composition x is adjusted to produce the desired transition temperature. We discuss design considerations and material choices, and present numerical simulations of the thermal response.

  19. Differential and total M-shell X-ray production cross-sections of some selected elements between Au and U at 5.96 keV

    International Nuclear Information System (INIS)

    Ozdemir, Yueksel

    2007-01-01

    Differential M-shell X-ray production (MXRP) cross-sections for selected heavy elements between Au and U have been measured at 5.59 keV incident photon energy, respectively at seven angles varying from 120 o to 150 o a Si(Li) detector. The differential M-shell X-ray production cross-sections have been derived, using M-shell fluorescence yields, experimental total M X-ray production cross-sections and theoretical M-shell photoionization cross-sections. The differential M-shell X-ray production cross-sections have been compared with the semi-empirical fits. The measured differential M X-ray production cross-sections have been found within experimental error. Differential M X-ray production cross-section can be fitted to the Σ n a n Z n (n = 2) as a function of cos θ. Total M X-ray production cross-sections have been derived using the fitted values

  20. Genetic algorithm using independent component analysis in x-ray reflectivity curve fitting of periodic layer structures

    International Nuclear Information System (INIS)

    Tiilikainen, J; Bosund, V; Tilli, J-M; Sormunen, J; Mattila, M; Hakkarainen, T; Lipsanen, H

    2007-01-01

    A novel genetic algorithm (GA) utilizing independent component analysis (ICA) was developed for x-ray reflectivity (XRR) curve fitting. EFICA was used to reduce mutual information, or interparameter dependences, during the combinatorial phase. The performance of the new algorithm was studied by fitting trial XRR curves to target curves which were computed using realistic multilayer models. The median convergence properties of conventional GA, GA using principal component analysis and the novel GA were compared. GA using ICA was found to outperform the other methods with problems having 41 parameters or more to be fitted without additional XRR curve calculations. The computational complexity of the conventional methods was linear but the novel method had a quadratic computational complexity due to the applied ICA method which sets a practical limit for the dimensionality of the problem to be solved. However, the novel algorithm had the best capability to extend the fitting analysis based on Parratt's formalism to multiperiodic layer structures

  1. X-ray View of Four High-Luminosity Swift-BAT AGN: Unveiling Obscuration and Reflection with Suzaku

    Science.gov (United States)

    Fiorettil, V.; Angelini, L.; Mushotzky, R. F.; Koss, M.; Malaguti, G.

    2013-01-01

    Aims. A complete census of obscured Active Galactic Nuclei (AGN) is necessary to reveal the history of the super massive black hole (SMBH) growth and galaxy evolution in the Universe given the complex feedback processes and the fact that much of this growth occurs in an obscured phase. In this context, hard X-ray surveys and dedicated follow-up observations represent a unique tool for selecting highly absorbed AGN and for characterizing the obscuring matter surrounding the SMBH. Here we focus on the absorption and reflection occurring in highly luminous, quasar-like AGN, to study the relation between the geometry of the absorbing matter and the AGN nature (e.g. X-ray, optical, and radio properties), and to help to determine the column density dependency on the AGN luminosity. Methods. The Swift/BAT nine-month survey observed 153 AGN, all with ultra-hard X-ray BAT fluxes in excess of 10(exp -11) erg per square centimeter and an average redshift of 0.03. Among them, four of the most luminous BAT AGN (44.73 less than LogLBAT less than 45.31) were selected as targets of Suzaku follow-up observations: J2246.0+3941 (3C 452), J0407.4+0339 (3C 105), J0318.7+6828, and J0918.5+0425. The column density, scattered/reflected emission, the properties of the Fe K line, and a possible variability are fully analyzed. For the latter, the spectral properties from Chandra, XMM-Newton and Swift/XRT public observations were compared with the present Suzaku analysis, adding an original spectral analysis when non was available from the literature. Results. Of our sample, 3C 452 is the only certain Compton-thick AGN candidate because of i) the high absorption (N(sub H) approximately 4 × 10(exp 23) per square centimeter) and strong Compton reflection; ii) the lack of variability; iii) the "buried" nature, i.e. the low scattering fraction (less than 0.5%) and the extremely low relative [OIII] luminosity. In contrast 3C 105 is not reflection-dominated, despite the comparable column density

  2. The polarized neutron reflectivity and X-ray reflectivity studies of the magnetic profiles of epitaxial Ni80Fe20/Ru multilayers

    International Nuclear Information System (INIS)

    Su, H.-C.; Peir, J.-J.; Lee, C.-H.; Lin, M.-Z.; Wu, P.-T.; Huang, J.C.A.; Tun Zin

    2005-01-01

    The depth profiles of the epitaxial Ni 80 Fe 20 (1 1 1)/Ru(0 0 0 1) multilayers were studied by polarized neutron reflectivity and X-ray reflectivity. At the Ru thickness that the anti-ferromagnetic coupling was found, the magnetic moments between two Ni 80 Fe 20 interlayers show a biquadratic coupling effect with a double unit cell at low applied fields. A magnetic dead layer of about 0.3 nm was also found at the interface boundaries. The maximal polarization effect applied to the Ru layer is less than 0.03μ B

  3. Synchrotron measurement of the 3D shape of X-ray reflections from the {gamma}/{gamma}{sup '}-microstructure of nickel-base superalloys

    Energy Technology Data Exchange (ETDEWEB)

    Epishin, Alexander; Link, Thomas; Ulbricht, Alexander; Bansal, Mamta [Technical Univ. of Berlin (Germany). Inst. of Material Science and Technology; Zizak, Ivo [Helmholtz-Zentrum Berlin for Materials and Energy BESSY II, Berlin (Germany)

    2011-12-15

    The 3D shape of X-ray reflections from the {gamma}/{gamma}{sup '}-microstructure of a nickel-base superalloy was investigated using synchrotron X-ray radiation and a position sensitive area detector. The measurements were performed on the 4{sup th} generation single-crystal nickel-base superalloy TMS138. The results show that X-ray reflections from non-cubic crystallographic planes have a complex 3D shape which changes during rafting. The 3D intensity distributions contain information about the spacing of the planes and their orientation as well. Whereas h00 reflections show the usual splitting into a {gamma}{sup '} and one {gamma}-subreflection, the hh0 and hhh reflections show two and three {gamma}-peaks respectively, resulting from the different types of {l_brace}100{r_brace} matrix channels. Therefore, these 3D diffraction measurements supply additional information about the spatial distribution of microstrains. (orig.)

  4. Determination of total iron in iron ore by x-ray fluorescence analysis using the Compton effect: comparison with others analytical techniques

    International Nuclear Information System (INIS)

    Castilho, M.V. de; Oliveira, R.C.

    1991-01-01

    Total iron in iron ores is determines by X-ray fluorescence analysis method using the compton effect. The Bragg angle is determined for compton no-coherent scattering related to K alpha of Rhodium. This measurement procedure can be used for best fitting of analytical results in X-ray fluorescence, when compared with others methods used for results corrections. (M.V.M.)

  5. X-ray reflectivity study of bias graded diamond like carbon film ...

    Indian Academy of Sciences (India)

    destructive technique for determining layer thickness, sur- face and interfacial roughness and internal structure of films. The XRR technique is alike the optical reflectivity technique and is performed at a glancing angle. ..... critical incident energy window the film attains minimum roughness. Thereafter, for higher energy the ...

  6. Biblical Poetry as Ethical Reflection: An X-Ray | Nmah | UJAH ...

    African Journals Online (AJOL)

    UJAH: Unizik Journal of Arts and Humanities. Journal Home · ABOUT THIS JOURNAL · Advanced Search · Current Issue · Archives · Journal Home > Special Edition 2011 >. Log in or Register to get access to full text downloads. Username, Password, Remember me, or Register. Biblical Poetry as Ethical Reflection: An X- ...

  7. Fourier X-ray line shape analysis of lattice defects from a single reflection

    International Nuclear Information System (INIS)

    Misra, N.K.; Bhanumurthy, K.

    1981-01-01

    A method of single reflection Fourier analysis has been described considering the fact that the rms strain (averaged over a distance) is not independent of averaging distance. Following the procedure of N.K. Misra and T.B. Ghosh (1976) and considering the initial slopes of dAsub(L)/dL against L curves, (Asub(L) is the Lsub(th) order Fourier coefficient) the effective size of the coherently diffracting domains and the rms strain in them are determined. The results of this analysis for pure Ti and Ag-3.55% Ga, Ag-15% In and Cu-12.46% Ge alloys compare fairly well with those obtained from different multiple reflections techniques. (author)

  8. The Effects of High Density on the X-ray Spectrum Reflected from Accretion Discs Around Black Holes

    Science.gov (United States)

    Garcia, Javier A.; Fabian, Andrew C.; Kallman, Timothy R.; Dauser, Thomas; Parker, Micahel L.; McClintock, Jeffrey E.; Steiner, James F.; Wilms, Jorn

    2016-01-01

    Current models of the spectrum of X-rays reflected from accretion discs around black holes and other compact objects are commonly calculated assuming that the density of the disc atmosphere is constant within several Thomson depths from the irradiated surface. An important simplifying assumption of these models is that the ionization structure of the gas is completely specified by a single, fixed value of the ionization parameter (xi), which is the ratio of the incident flux to the gas density. The density is typically fixed at n(sub e) = 10(exp 15) per cu cm. Motivated by observations, we consider higher densities in the calculation of the reflected spectrum. We show by computing model spectra for n(sub e) approximately greater than 10(exp 17) per cu cm that high-density effects significantly modify reflection spectra. The main effect is to boost the thermal continuum at energies 2 approximately less than keV. We discuss the implications of these results for interpreting observations of both active galactic nuclei and black hole binaries. We also discuss the limitations of our models imposed by the quality of the atomic data currently available.

  9. ON ESTIMATING THE HIGH-ENERGY CUTOFF IN THE X-RAY SPECTRA OF BLACK HOLES VIA REFLECTION SPECTROSCOPY

    Energy Technology Data Exchange (ETDEWEB)

    García, Javier A.; Steiner, James F.; McClintock, Jeffrey E.; Keck, Mason L. [Harvard-Smithsonian Center for Astrophysics, 60 Garden St., Cambridge, MA 02138 (United States); Dauser, Thomas; Wilms, Jörn, E-mail: javier@head.cfa.harvard.edu, E-mail: jem@cfa.harvard.edu, E-mail: jsteiner@head.cfa.harvard.edu, E-mail: keckm@bu.edu, E-mail: thomas.dauser@sternwarte.uni-erlangen.de [Dr. Karl Remeis-Observatory and Erlangen Centre for Astroparticle Physics, Sternwartstr. 7, D-96049 Bamberg (Germany)

    2015-08-01

    The fundamental parameters describing the coronal spectrum of an accreting black hole are the slope Γ of the power-law continuum and the energy E{sub cut} at which it rolls over. Remarkably, this latter parameter can be accurately measured for values as high as 1 MeV by modeling the spectrum of X-rays reflected from a black hole accretion disk at energies below 100 keV. This is possible because the details in the reflection spectrum, rich in fluorescent lines and other atomic features, are very sensitive to the spectral shape of the hardest coronal radiation illuminating the disk. We show that by fitting simultaneous NuSTAR (3–79 keV) and low-energy (e.g., Suzaku) data with the most recent version of our reflection model relxill one can obtain reasonable constraints on E{sub cut} at energies from tens of keV up to 1 MeV, for a source as faint as 1 mCrab in a 100 ks observation.

  10. Multi-layer thickness determination using differential-based enhanced Fourier transforms of X-ray reflectivity data

    Energy Technology Data Exchange (ETDEWEB)

    Poust, Benjamin [Department of Materials Science and Engineering, University of California, Los Angeles, CA (United States); Northrop Grumman Space Technology, Redondo Beach, CA (United States); Sandhu, Rajinder [Northrop Grumman Space Technology, Redondo Beach, CA (United States); Goorsky, Mark [Department of Materials Science and Engineering, University of California, Los Angeles, CA (United States)

    2009-08-15

    Layer thickness determination of single and multi-layer structures is achieved using a new method for generating Fourier transforms (FTs) of X-ray reflectivity data. This enhanced Fourier analysis is compared to other techniques in the determination of AlN layer thickness deposited on sapphire. In addition to demonstrably improved results, the results also agree with thicknesses determined using simulations and TEM measurements. The effectiveness of the technique is further demonstrated using the more complicated metamorphic epitaxial multi-layer AlSb/InAs structures deposited on GaAs. The approach reported here is based upon differentiating the specular intensity with respect to the vertical reciprocal space coordinate Q{sub Z}. In general, differentiation is far more effective at removing the sloping background present in reflectivity scans than logarithmic compression alone, average subtraction alone, or other methods. When combined with any of the other enhancement techniques, however, differentiation yields distinguishable discrete Fourier transform (DFT) power spectrum peaks for even the weakest and most truncated of sloping oscillations that are present in many reflectivity scans from multi-layer structures. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  11. Influence of a carbon over-coat on the X-ray reflectance of XEUS mirrors

    DEFF Research Database (Denmark)

    Lumb, D.H.; Christensen, Finn Erland; Cooper-Jensen, Carsten P.

    2007-01-01

    , with that for samples with an additional 10 nm thick carbon over-coating. We demonstrate a significant improvement in reflectance in the energy range similar to 1-4 keV, and at a grazing incidence angle of 10 mrad (0.57 degrees). We consider the resulting effective area that could be attained with an optimized design...... of the XEUS telescope. Typically an improvement of 10-60% in effective area, depending on photon energy, can be achieved using the carbon overcoat....

  12. Superradiance or total reflection?

    CERN Document Server

    László, András

    2014-01-01

    Numerical evolution of massless scalar fields on Kerr background is studied. The initial data specifications are chosen to have compact support separated from the ergoregion and to yield nearly monochromatic incident wave packets. The initial data is also tuned to maximize the effect of superradiance. Evidences are shown indicating that instead of the anticipated energy extraction from black hole the incident radiation fail to reach the ergoregion rather it suffers a nearly perfect reflection.

  13. Synchrotron radiation total reflection for rainwater analysis

    International Nuclear Information System (INIS)

    Simabuco, Silvana M.; Matsumoto, Edson

    1999-01-01

    Total reflection X-ray fluorescence analysis excited with synchrotron radiation (SR-TXRF) has been used for rainwater trace element analysis. The samples were collected in four different sites at Campinas City, SP. Standard solutions with gallium as internal standard were prepared for the calibration system. Rainwater samples of 10 μl were putted onto Perspex reflector disk, dried on vacuum and analyzed for 100 s measuring time. The detection limits obtained for K-shell varied from 29 ng.ml -1 for sulfur to 1.3 ng.ml -1 for zinc and copper, while for L-shell the values were 4.5 ng.ml -1 for mercury and 7.0 ng.ml -1 for lead. (author)

  14. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction; Nouvelles etudes structurales de cristaux liquides par reflectivite et diffraction resonante des rayons X

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, P

    2007-04-15

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B{sub 2} liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B{sub 2} phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation.

  15. Dynamic re-weighted total variation technique and statistic Iterative reconstruction method for x-ray CT metal artifact reduction

    Science.gov (United States)

    Peng, Chengtao; Qiu, Bensheng; Zhang, Cheng; Ma, Changyu; Yuan, Gang; Li, Ming

    2017-07-01

    Over the years, the X-ray computed tomography (CT) has been successfully used in clinical diagnosis. However, when the body of the patient to be examined contains metal objects, the image reconstructed would be polluted by severe metal artifacts, which affect the doctor's diagnosis of disease. In this work, we proposed a dynamic re-weighted total variation (DRWTV) technique combined with the statistic iterative reconstruction (SIR) method to reduce the artifacts. The DRWTV method is based on the total variation (TV) and re-weighted total variation (RWTV) techniques, but it provides a sparser representation than TV and protects the tissue details better than RWTV. Besides, the DRWTV can suppress the artifacts and noise, and the SIR convergence speed is also accelerated. The performance of the algorithm is tested on both simulated phantom dataset and clinical dataset, which are the teeth phantom with two metal implants and the skull with three metal implants, respectively. The proposed algorithm (SIR-DRWTV) is compared with two traditional iterative algorithms, which are SIR and SIR constrained by RWTV regulation (SIR-RWTV). The results show that the proposed algorithm has the best performance in reducing metal artifacts and protecting tissue details.

  16. Skull x-ray

    Science.gov (United States)

    X-ray - head; X-ray - skull; Skull radiography; Head x-ray ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  17. Neck x-ray

    Science.gov (United States)

    X-ray - neck; Cervical spine x-ray; Lateral neck x-ray ... There is low radiation exposure. X-rays are monitored so that the lowest amount of radiation is used to produce the image. Pregnant women and ...

  18. Direct and inverse problems of studying the properties of multilayer nanostructures based on a two-dimensional model of X-ray reflection and scattering

    Science.gov (United States)

    Khachaturov, R. V.

    2014-06-01

    A mathematical model of X-ray reflection and scattering by multilayered nanostructures in the quasi-optical approximation is proposed. X-ray propagation and the electric field distribution inside the multilayered structure are considered with allowance for refraction, which is taken into account via the second derivative with respect to the depth of the structure. This model is used to demonstrate the possibility of solving inverse problems in order to determine the characteristics of irregularities not only over the depth (as in the one-dimensional problem) but also over the length of the structure. An approximate combinatorial method for system decomposition and composition is proposed for solving the inverse problems.

  19. On the Determination of the Spin of the Black Hole in Cyg X-1 from X-Ray Reflection Spectra

    Science.gov (United States)

    Fabian, A. C.; Wilkins, D.; Miller, J. M.; Reis, R. C.; Reynolds, C. S.; Cackett, E. M.; Nowak, M. A.; Pooley, G.; Pottschmidt, K.; Sanders, J. S.; hide

    2012-01-01

    The spin of Cygnus X-I is measured by fitting reflection models to Suzaku data covering the energy band 0.9-400 keY. The inner radius of the accretion disc is found to lie within 2 gravitational radii (rg = GM/c(exp 2)) and a value for the dimensionless black hole spin is obtained of 0.97(sup .0.14) (sup -0.02). This agrees with recent measurements using the continuum fitting method by Gou et al. and of the broad iron line by Duro et al. The disc inclination is measured at 23.7(sup +6.7) (sup -5.4) deg. which is consistent with the recent optical measurement of the binary system inclination by Orosz et al of 27+/- 0.8 deg. We pay special attention to the emissivity profile caused by irradiation of the inner disc by the hard power-law source. 1be X-ray observations and simulations show that the index q of that profile deviates from the commonly used, Newtonian, value of 3 within 3r(sub g), steepening considerably within 2r(sub g). as expected in the strong gravity regime.

  20. Fitness function and nonunique solutions in x-ray reflectivity curve fitting: crosserror between surface roughness and mass density

    International Nuclear Information System (INIS)

    Tiilikainen, J; Bosund, V; Mattila, M; Hakkarainen, T; Sormunen, J; Lipsanen, H

    2007-01-01

    Nonunique solutions of the x-ray reflectivity (XRR) curve fitting problem were studied by modelling layer structures with neural networks and designing a fitness function to handle the nonidealities of measurements. Modelled atomic-layer-deposited aluminium oxide film structures were used in the simulations to calculate XRR curves based on Parratt's formalism. This approach reduced the dimensionality of the parameter space and allowed the use of fitness landscapes in the study of nonunique solutions. Fitness landscapes, where the height in a map represents the fitness value as a function of the process parameters, revealed tracks where the local fitness optima lie. The tracks were projected on the physical parameter space thus allowing the construction of the crosserror equation between weakly determined parameters, i.e. between the mass density and the surface roughness of a layer. The equation gives the minimum error for the other parameters which is a consequence of the nonuniqueness of the solution if noise is present. Furthermore, the existence of a possible unique solution in a certain parameter range was found to be dependent on the layer thickness and the signal-to-noise ratio

  1. Combined evaluation of grazing incidence X-ray fluorescence and X-ray reflectivity data for improved profiling of ultra-shallow depth distributions

    NARCIS (Netherlands)

    Ingerle, D.; Meirer, F.; Pepponi, G.; Demenev, E.; Giubertoni, D.; Wobrauschek, P.; Streli, C.

    2014-01-01

    The continuous downscaling of the process size for semiconductor devices pushes the junction depths and consequentially the implantation depths to the top few nanometers of the Si substrate. This motivates the need for sensitive methods capable of analyzing dopant distribution, total dose and

  2. Total and regional bone mineral content in healthy Spanish subjects by dual-energy X-ray absorptiometry

    International Nuclear Information System (INIS)

    Aguado Henche, S.; Rodriguez Torres, R.; Clemente de Arriba, C.; Gomez Pellico, L.

    2008-01-01

    This is an observational cross-sectional study. The aim of the present study was to describe and analyze patterns of change in total and regional bone mineral content in relation to age and gender in a sedentary Spanish sample population (from the Community of Madrid). The age range of the sample population was from birth to 80 years. One thousand one hundred twenty healthy subjects were recruited and divided into 16 groups according to age. Each subject underwent whole-body densitometry using dual-energy X-ray absorptiometry. An analysis was made of the amount of bone mineral content (BMC) in the whole body and in different regions: the head, trunk, upper limbs, and lower limbs. Gender differences in mean values for upper limbs and lower limbs are statistically significant between 16 and 70 years of age. For the head and trunk, the mean BMC values show the most significant gender differences between 16 and 25 years of age (p≤0.001). Total bone mineral content (TBMC) and TBMC-to-height ratio show significant gender differences between 16 and 70 years of age. In females, TBMC values increase up to 20 years of age and in males up to 25 years of age. We have determined an evolutionary normal pattern of bone mineral content in urban Spanish people. (orig.)

  3. Total and regional bone mineral content in healthy Spanish subjects by dual-energy X-ray absorptiometry

    Energy Technology Data Exchange (ETDEWEB)

    Aguado Henche, S.; Rodriguez Torres, R.; Clemente de Arriba, C.; Gomez Pellico, L. [Universidad de Alcala, Departamento de Anatomia y Embriologia Humana, Facultad de Medicina, Alcala de Henares, Madrid (Spain)

    2008-11-15

    This is an observational cross-sectional study. The aim of the present study was to describe and analyze patterns of change in total and regional bone mineral content in relation to age and gender in a sedentary Spanish sample population (from the Community of Madrid). The age range of the sample population was from birth to 80 years. One thousand one hundred twenty healthy subjects were recruited and divided into 16 groups according to age. Each subject underwent whole-body densitometry using dual-energy X-ray absorptiometry. An analysis was made of the amount of bone mineral content (BMC) in the whole body and in different regions: the head, trunk, upper limbs, and lower limbs. Gender differences in mean values for upper limbs and lower limbs are statistically significant between 16 and 70 years of age. For the head and trunk, the mean BMC values show the most significant gender differences between 16 and 25 years of age (p{<=}0.001). Total bone mineral content (TBMC) and TBMC-to-height ratio show significant gender differences between 16 and 70 years of age. In females, TBMC values increase up to 20 years of age and in males up to 25 years of age. We have determined an evolutionary normal pattern of bone mineral content in urban Spanish people. (orig.)

  4. Change in fat-free mass assessed by bioelectrical impedance, total body potassium and dual energy X-ray absorptiometry during prolonged weight loss

    DEFF Research Database (Denmark)

    Hendel, H W; Gotfredsen, A; Højgaard, L

    1996-01-01

    A total of 16 obese women (body mass index (BMI) 30-43 kg m(-2)) participated in a weight reduction study. Before and after a weight loss of 11.7 +/- 7.4 kg (mean +/- SD), body composition was assessed by dual energy X-ray absorptiometry (DXA), and total body potassium counting (TBK). These measu...

  5. X-Ray Reflection and an Exceptionally Long Thermonuclear Helium Burst from IGR J17062-6143

    Energy Technology Data Exchange (ETDEWEB)

    Keek, L.; Strohmayer, T. E. [X-ray Astrophysics Laboratory, Astrophysics Science Division, NASA/GSFC, Greenbelt, MD 20771 (United States); Iwakiri, W.; Serino, M. [MAXI team, RIKEN, 2-1 Hirosawa, Wako, Saitama 351-0198 (Japan); Ballantyne, D. R. [Center for Relativistic Astrophysics, School of Physics, Georgia Institute of Technology, 837 State Street, Atlanta, GA 30332-0430 (United States); Zand, J. J. M. in’t, E-mail: laurens.keek@nasa.gov [SRON Netherlands Institute for Space Research, Sorbonnelaan 2, 3584 CA Utrecht (Netherlands)

    2017-02-10

    Thermonuclear X-ray bursts from accreting neutron stars power brief but strong irradiation of their surroundings, providing a unique way to study accretion physics. We analyze MAXI /Gas Slit Camera and Swift /XRT spectra of a day-long flash observed from IGR J17062-6143 in 2015. It is a rare case of recurring bursts at a low accretion luminosity of 0.15% Eddington. Spectra from MAXI , Chandra , and NuSTAR observations taken between the 2015 burst and the previous one in 2012 are used to determine the accretion column. We find it to be consistent with the burst ignition column of 5×10{sup 10} g cm{sup −2}, which indicates that it is likely powered by burning in a deep helium layer. The burst flux is observed for over a day, and decays as a straight power law: F ∝ t {sup −1.15}. The burst and persistent spectra are well described by thermal emission from the neutron star, Comptonization of this emission in a hot optically thin medium surrounding the star, and reflection off the photoionized accretion disk. At the burst peak, the Comptonized component disappears, when the burst may dissipate the Comptonizing gas, and it returns in the burst tail. The reflection signal suggests that the inner disk is truncated at ∼10{sup 2} gravitational radii before the burst, but may move closer to the star during the burst. At the end of the burst, the flux drops below the burst cooling trend for 2 days, before returning to the pre-burst level.

  6. Moments of the Bethe surface and total inelastic x-ray scattering cross sections for H2

    International Nuclear Information System (INIS)

    Sharma, B.S.; Thakkar, A.J.

    1987-01-01

    Moments, S(j,K), of the generalized oscillator strength distribution are global properties of the Bethe surface. Apart from S(-1,K) which is related to the Waller-Hartree incoherent scattering factor, little is known about these moments for nonzero K. This paper describes high-accuracy calculations of S(1,K) and S(2,K) for molecular hydrogen. Comparison with experiment is made, and the utility of simple asymptotic approximations is confirmed. The moments are used to calculate differential cross sections for the inelastic scattering of x rays using the constant-momentum-transfer and constant-angle theories of Bonham. These cross sections differ from the Waller-Hartree cross sections at large angles thus demonstrating the importance of making corrections to the Waller-Hartree theory if the incoherent scattering factor S(K) is to be extracted from experimental inelastic cross sections. Total cross sections for scattering of 6- and 7-keV photons from H 2 are compared with synchrotron radiation scattering experiments. The calculations suggest that the Bonham constant-angle cross sections agree best with experiment. However, further experimental and theoretical work is needed to obtain firm conclusions about the limitations of Waller-Hartree theory

  7. Real-time fusion of coronary CT angiography with X-ray fluoroscopy during chronic total occlusion PCI

    Energy Technology Data Exchange (ETDEWEB)

    Ghoshhajra, Brian B.; Takx, Richard A.P. [Harvard Medical School, Cardiac MR PET CT Program, Massachusetts General Hospital, Department of Radiology and Division of Cardiology, Boston, MA (United States); Stone, Luke L.; Yeh, Robert W.; Jaffer, Farouc A. [Harvard Medical School, Cardiac Cathetrization Laboratory, Cardiology Division, Massachusetts General Hospital, Boston, MA (United States); Girard, Erin E. [Siemens Healthcare, Princeton, NJ (United States); Brilakis, Emmanouil S. [Cardiology Division, Dallas VA Medical Center and UT Southwestern Medical Center, Dallas, TX (United States); Lombardi, William L. [University of Washington, Cardiology Division, Seattle, WA (United States)

    2017-06-15

    The purpose of this study was to demonstrate the feasibility of real-time fusion of coronary computed tomography angiography (CTA) centreline and arterial wall calcification with X-ray fluoroscopy during chronic total occlusion (CTO) percutaneous coronary intervention (PCI). Patients undergoing CTO PCI were prospectively enrolled. Pre-procedural CT scans were integrated with conventional coronary fluoroscopy using prototype software. We enrolled 24 patients who underwent CTO PCI using the prototype CT fusion software, and 24 consecutive CTO PCI patients without CT guidance served as a control group. Mean age was 66 ± 11 years, and 43/48 patients were men. Real-time CTA fusion during CTO PCI provided additional information regarding coronary arterial calcification and tortuosity that generated new insights into antegrade wiring, antegrade dissection/reentry, and retrograde wiring during CTO PCI. Overall CTO success rates and procedural outcomes remained similar between the two groups, despite a trend toward higher complexity in the fusion CTA group. This study demonstrates that real-time automated co-registration of coronary CTA centreline and calcification onto live fluoroscopic images is feasible and provides new insights into CTO PCI, and in particular, antegrade dissection reentry-based CTO PCI. (orig.)

  8. Adaptive-weighted total variation minimization for sparse data toward low-dose x-ray computed tomography image reconstruction.

    Science.gov (United States)

    Liu, Yan; Ma, Jianhua; Fan, Yi; Liang, Zhengrong

    2012-12-07

    Previous studies have shown that by minimizing the total variation (TV) of the to-be-estimated image with some data and other constraints, piecewise-smooth x-ray computed tomography (CT) can be reconstructed from sparse-view projection data without introducing notable artifacts. However, due to the piecewise constant assumption for the image, a conventional TV minimization algorithm often suffers from over-smoothness on the edges of the resulting image. To mitigate this drawback, we present an adaptive-weighted TV (AwTV) minimization algorithm in this paper. The presented AwTV model is derived by considering the anisotropic edge property among neighboring image voxels, where the associated weights are expressed as an exponential function and can be adaptively adjusted by the local image-intensity gradient for the purpose of preserving the edge details. Inspired by the previously reported TV-POCS (projection onto convex sets) implementation, a similar AwTV-POCS implementation was developed to minimize the AwTV subject to data and other constraints for the purpose of sparse-view low-dose CT image reconstruction. To evaluate the presented AwTV-POCS algorithm, both qualitative and quantitative studies were performed by computer simulations and phantom experiments. The results show that the presented AwTV-POCS algorithm can yield images with several notable gains, in terms of noise-resolution tradeoff plots and full-width at half-maximum values, as compared to the corresponding conventional TV-POCS algorithm.

  9. Real-time fusion of coronary CT angiography with x-ray fluoroscopy during chronic total occlusion PCI.

    Science.gov (United States)

    Ghoshhajra, Brian B; Takx, Richard A P; Stone, Luke L; Girard, Erin E; Brilakis, Emmanouil S; Lombardi, William L; Yeh, Robert W; Jaffer, Farouc A

    2017-06-01

    The purpose of this study was to demonstrate the feasibility of real-time fusion of coronary computed tomography angiography (CTA) centreline and arterial wall calcification with x-ray fluoroscopy during chronic total occlusion (CTO) percutaneous coronary intervention (PCI). Patients undergoing CTO PCI were prospectively enrolled. Pre-procedural CT scans were integrated with conventional coronary fluoroscopy using prototype software. We enrolled 24 patients who underwent CTO PCI using the prototype CT fusion software, and 24 consecutive CTO PCI patients without CT guidance served as a control group. Mean age was 66 ± 11 years, and 43/48 patients were men. Real-time CTA fusion during CTO PCI provided additional information regarding coronary arterial calcification and tortuosity that generated new insights into antegrade wiring, antegrade dissection/reentry, and retrograde wiring during CTO PCI. Overall CTO success rates and procedural outcomes remained similar between the two groups, despite a trend toward higher complexity in the fusion CTA group. This study demonstrates that real-time automated co-registration of coronary CTA centreline and calcification onto live fluoroscopic images is feasible and provides new insights into CTO PCI, and in particular, antegrade dissection reentry-based CTO PCI. • Real-time semi-automated fusion of CTA/fluoroscopy is feasible during CTO PCI. • CTA fusion data can be toggled on/off as desired during CTO PCI • Real-time CT calcium and centreline overlay could benefit antegrade dissection/reentry-based CTO PCI.

  10. Cobalt coordination and clustering in alpha-Co(OH)(2) revealed by synchrotron X-ray total scattering.

    Science.gov (United States)

    Neilson, James R; Kurzman, Joshua A; Seshadri, Ram; Morse, Daniel E

    2010-09-03

    Structures of layered metal hydroxides are not well described by traditional crystallography. Total scattering from a synthesis-controlled subset of these materials, as described here, reveals that different cobalt coordination polyhedra cluster within each layer on short length scales, offering new insights and approaches for understanding the properties of these and related layered materials. Structures related to that of brucite [Mg(OH)(2)] are ubiquitous in the mineral world and offer a variety of useful functions ranging from catalysis and ion-exchange to sequestration and energy transduction, including applications in batteries. However, it has been difficult to resolve the atomic structure of these layered compounds because interlayer disorder disrupts the long-range periodicity necessary for diffraction-based structure determination. For this reason, traditional unit-cell-based descriptions have remained inaccurate. Here we apply, for the first time to such layered hydroxides, synchrotron X-ray total scattering methods-analyzing both the Bragg and diffuse components-to resolve the intralayer structure of three different alpha-cobalt hydroxides, revealing the nature and distribution of metal site coordination. The different compounds with incorporated chloride ions have been prepared with kinetic control of hydrolysis to yield different ratios of octahedrally and tetrahedrally coordinated cobalt ions within the layers, as confirmed by total scattering. Real-space analyses indicate local clustering of polyhedra within the layers, manifested in the weighted average of different ordered phases with fixed fractions of tetrahedrally coordinated cobalt sites. These results, hidden from an averaged unit-cell description, reveal new structural characteristics that are essential to understanding the origin of fundamental material properties such as color, anion exchange capacity, and magnetic behavior. Our results also provide further insights into the detailed

  11. Cobalt Coordination and Clustering in α-Co(OH)2 Revealed by Synchrotron X-ray Total Scattering

    International Nuclear Information System (INIS)

    Neilson, James R.; Kurzman, Joshua A.; Seshadri, Ram; Morse, Daniel E.

    2010-01-01

    Structures of layered metal hydroxides are not well described by traditional crystallography. Total scattering from a synthesis-controlled subset of these materials, as described here, reveals that different cobalt coordination polyhedra cluster within each layer on short length scales, offering new insights and approaches for understanding the properties of these and related layered materials. Structures related to that of brucite (Mg(OH) 2 ) are ubiquitous in the mineral world and offer a variety of useful functions ranging from catalysis and ion-exchange to sequestration and energy transduction, including applications in batteries. However, it has been difficult to resolve the atomic structure of these layered compounds because interlayer disorder disrupts the long-range periodicity necessary for diffraction-based structure determination. For this reason, traditional unit-cell-based descriptions have remained inaccurate. Here we apply, for the first time to such layered hydroxides, synchrotron X-ray total scattering methods - analyzing both the Bragg and diffuse components - to resolve the intralayer structure of three different α-cobalt hydroxides, revealing the nature and distribution of metal site coordination. The different compounds with incorporated chloride ions have been prepared with kinetic control of hydrolysis to yield different ratios of octahedrally and tetrahedrally coordinated cobalt ions within the layers, as confirmed by total scattering. Real-space analyses indicate local clustering of polyhedra within the layers, manifested in the weighted average of different ordered phases with fixed fractions of tetrahedrally coordinated cobalt sites. These results, hidden from an averaged unit-cell description, reveal new structural characteristics that are essential to understanding the origin of fundamental material properties such as color, anion exchange capacity, and magnetic behavior. Our results also provide further insights into the detailed

  12. Impact of Lipid Oxidization on Vertical Structures and Electrostatics of Phospholipid Monolayers Revealed by Combination of Specular X-ray Reflectivity and Grazing-Incidence X-ray Fluorescence.

    Science.gov (United States)

    Korytowski, Agatha; Abuillan, Wasim; Makky, Ali; Konovalov, Oleg; Tanaka, Motomu

    2015-07-30

    The influence of phospholipid oxidization of floating monolayers on the structure perpendicular to the global plane and on the density profiles of ions near the lipid monolayer has been investigated by a combination of grazing incidence X-ray fluorescence (GIXF) and specular X-ray reflectivity (XRR). Systematic variation of the composition of the floating monolayers unravels changes in the thickness, roughness and electron density of the lipid monolayers as a function of molar fraction of oxidized phospholipids. Simultaneous GIXF measurements enable one to qualitatively determine the element-specific density profiles of monovalent (K(+) or Cs(+)) and divalent ions (Ca(2+)) in the vicinity of the interface in the presence and absence of two types of oxidized phospholipids (PazePC and PoxnoPC) with high spatial accuracy (±5 Å). We found the condensation of Ca(2+) near carboxylated PazePC was more pronounced compared to PoxnoPC with an aldehyde group. In contrast, the condensation of monovalent ions could hardly be detected even for pure oxidized phospholipid monolayers. Moreover, pure phospholipid monolayers exhibited almost no ion specific condensation near the interface. The quantitative studies with well-defined floating monolayers revealed how the elevation of lipid oxidization level alters the structures and functions of cell membranes.

  13. Radiation doses for X-ray diagnosis teeth in dental medicine

    International Nuclear Information System (INIS)

    Direkov, Lyubomir

    2009-01-01

    X-rays are the first ionizing radiation, which are applied in medicine for diagnostic radiology and X-ray therapy. While in the beginning they are mainly used for X-ray photos of the chest /lungs and in severe fractures of the limbs, then in recent years they are widely applied in diagnostics of teeth in dental medicine. Considering that caries is a widespread disease, both in children and adults, and it requires repeated x-ray photographs of the damaged teeth for the individual, the total radiation doses, which reflect on people from the X-rays are at high values. In order to reduce external exposure to other organs /mainly thyroid gland/ by X-ray pictures of teeth, it should be used with special lead aprons with large coefficient of reduction. Keywords: doses of radiation, X-ray machines, dental, x-ray pictures of teeth, protection sources

  14. 3D reconstruction of pentacene structural organization in top-contact OTFTs via resonant soft X-ray reflectivity

    Science.gov (United States)

    Capelli, Raffaella; Nardi, Marco Vittorio; Toccoli, Tullio; Verucchi, Roberto; Dinelli, Franco; Gelsomini, Carolina; Koshmak, Konstantin; Giglia, Angelo; Nannarone, Stefano; Pasquali, Luca

    2018-01-01

    Herein, we describe the use of soft X-ray reflectivity at the carbon K-edge to study the molecular organization (orientation, structure, and morphology) of pentacene active films in a top-contact transistor geometry. This technique is not affected by sample charging, and it can be applied in the case of insulating substrates. In addition, the sampling depth is not limited to the near-surface region, giving access to buried device interfaces (metal/organic and dielectric/organic). Spectral lineshape simulations, based on ab-initio calculations using a realistic 3D layer-by-layer model, allow us to unravel the details of the molecular organization in all the specific and crucial areas of the active film, overcoming the limitations of conventional approaches. The tilt angle of the long molecular axis in the whole film is found to progressively decrease with respect to the substrate normal from 25° to 0° with the increasing film thickness. A full vertical alignment, optimal for in-plane charge hopping, is reached only after the complete formation of the first five monolayers. Remarkably, starting from the first one in contact with the dielectric substrate, all the monolayers in the stack show a change in orientation with the increasing thickness. On the other hand, at the buried interface with a gold top-contact, the molecules assume a flat orientation that only propagates for two or three monolayers into the organic film. Top-contact devices with the highest performances can thus be obtained using films of at least ten monolayers. This explains the observed thickness dependence of charge mobility in pentacene transistors.

  15. Method for spatially modulating X-ray pulses using MEMS-based X-ray optics

    Science.gov (United States)

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

    2015-03-10

    A method and apparatus are provided for spatially modulating X-rays or X-ray pulses using microelectromechanical systems (MEMS) based X-ray optics. A torsionally-oscillating MEMS micromirror and a method of leveraging the grazing-angle reflection property are provided to modulate X-ray pulses with a high-degree of controllability.

  16. Ultra-short-period W/B4C multilayers for x-ray optics-microstructure limits on reflectivity

    Energy Technology Data Exchange (ETDEWEB)

    Walton, Christopher Charles [Univ. of California, Berkeley, CA (United States). Dept. of Materials Science and Mineral Engineering

    1997-12-01

    Multilayer thin films are used as Bragg reflectors for soft x-rays in the energy range 50eV < E < 1000eV in many x-ray optics applications such as x-ray microscopes and telescopes, reducing optics for extreme ultraviolet (EUV) lithography, and x-ray polarizers and phase retarders. Applications often depend critically on reflectivity, which has not been systematically characterized for multilayer periods below 20Å. For this study, W/B4C multilayers were fabricated by magnetron sputtering on Si(111), with periods from 48Å to as little as 4.7Å. The x-ray reflectivity measured at λ = 1.54Å and at 45° incidence (289 eV < E < 860 eV) was found to decrease sharply for multilayer periods less than 15-20Å. Examination by high-resolution transmission electron microscopy (HRTEM) showed an expansion of the thickness of the W-rich layers of 30-40% from the nominal values, consistent with intermixture of the two materials during sputter growth, and discontinuous W-rich layers for multilayer periods below about 15Å. The experimental data for the specular reflectivity in the hard and soft x-ray regimes and the diffuse scattering fit well to a model of multilayer roughness. The model is expressed as a power-law dependence of roughness on spatial frequency. Analysis of small-angle scattering in transmission from multilayers grown on freestanding Si3N4 membranes confirms the onset of discontinuity at periods between 14Å and 22Å. Spectroscopy studies by x-ray absorption (NEXAFS) and electron energy loss (EELS) at the boron K-edge (188eV) are consistent with changes in the average boron bonding environment, as the multilayer period decreases and the W-rich layers are increasingly thin and dispersed. A discrete W-rich phase is present for periods at least as small as 6.3Å.

  17. The X-Ray Reflection Spectrum of the Radio-loud Quasar 4C 74.26

    DEFF Research Database (Denmark)

    Lohfink, Anne M.; Fabian, Andrew C.; Ballantyne, David R.

    2017-01-01

    of the supermassive black hole, the presumed jet launching point, are potentially particularly valuable in illuminating the jet formation process. Here, we present the hard X-ray NuSTAR observations of the radio-loud quasar 4C 74.26 in a joint analysis with quasi-simultaneous, soft X-ray Swift observations. Our...... the three months covered by our NuSTAR campaign. This lack of variation could mean that the jet formation in this radio-loud quasar differs from what is observed in broad-line radio galaxies....

  18. Capacity of X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Wobrauschek, P.; Kregsamer, P.

    1997-01-01

    X-Ray fluorescence analysis (XRF) is a powerful analytical tool for the qualitative and quantitative determination of chemical elements in a sample. Two different detection principles are accepted widely: wavelength dispersive and energy dispersive. Various sources for XRF are discussed: X-ray tubes, accelerators for particle induced XRF, radioactive isotopes, and the use of synchrotron radiation. Applications include environmental, technical, medical, fine art, and forensic studies. Due to the demands of research and application special techniques like total reflection XRF (TXRF) were developed with ultimately achievable detection limits in the femtogram region. The elements detectable by XRF range from Be to U. (author)

  19. The X-Ray Reflection Spectrum of the Radio-loud Quasar 4C 74.26

    DEFF Research Database (Denmark)

    Lohfink, Anne M.; Fabian, Andrew C.; Ballantyne, David R.

    2017-01-01

    The relativistic jets created by some active galactic nuclei are important agents of AGN feedback. In spite of this, our understanding of what produces these jets is still incomplete. X-ray observations, which can probe the processes operating in the central regions in the immediate vicinity of t...... the three months covered by our NuSTAR campaign. This lack of variation could mean that the jet formation in this radio-loud quasar differs from what is observed in broad-line radio galaxies.......The relativistic jets created by some active galactic nuclei are important agents of AGN feedback. In spite of this, our understanding of what produces these jets is still incomplete. X-ray observations, which can probe the processes operating in the central regions in the immediate vicinity...... of the supermassive black hole, the presumed jet launching point, are potentially particularly valuable in illuminating the jet formation process. Here, we present the hard X-ray NuSTAR observations of the radio-loud quasar 4C 74.26 in a joint analysis with quasi-simultaneous, soft X-ray Swift observations. Our...

  20. Nonlinear fitness-space-structure adaptation and principal component analysis in genetic algorithms: an application to x-ray reflectivity analysis

    International Nuclear Information System (INIS)

    Tiilikainen, J; Tilli, J-M; Bosund, V; Mattila, M; Hakkarainen, T; Airaksinen, V-M; Lipsanen, H

    2007-01-01

    Two novel genetic algorithms implementing principal component analysis and an adaptive nonlinear fitness-space-structure technique are presented and compared with conventional algorithms in x-ray reflectivity analysis. Principal component analysis based on Hessian or interparameter covariance matrices is used to rotate a coordinate frame. The nonlinear adaptation applies nonlinear estimates to reshape the probability distribution of the trial parameters. The simulated x-ray reflectivity of a realistic model of a periodic nanolaminate structure was used as a test case for the fitting algorithms. The novel methods had significantly faster convergence and less stagnation than conventional non-adaptive genetic algorithms. The covariance approach needs no additional curve calculations compared with conventional methods, and it had better convergence properties than the computationally expensive Hessian approach. These new algorithms can also be applied to other fitting problems where tight interparameter dependence is present

  1. Characteristics of soft X-ray lens

    International Nuclear Information System (INIS)

    Qin Yi

    2007-12-01

    A soft X-lens was devised with waveguide X-ray optics of total external reflection (TER). The lens consists of a stack of 1 387 TER waveguides with inner diameter of 0.45 mm and outer diameter of 0.60 mm. With the help of plasma sources of soft X-ray radiation, high density of pure soft X-ray radiation (without plasma expansion fragments) with broad-band spectral range can be obtained at the focus of the lens. As laser-plasma is considered, the radiation density of 1.3 x 10 5 W/cm 2 is obtained, the transmission coefficient is 18.6%, the ratio of the density at the focus with and without the lens is 1000 and the radiation capture is 28.9 degree. The density of 0.5 TW/cm 2 can be obtained as far as Qiang-Guang I facility is considered. (authors)

  2. X-Ray

    Science.gov (United States)

    ... enema. What you can expect During the X-ray X-rays are performed at doctors' offices, dentists' offices, ... as those using a contrast medium. Your child's X-ray Restraints or other techniques may be used to ...

  3. Abdominal x-ray

    Science.gov (United States)

    Abdominal film; X-ray - abdomen; Flat plate; KUB x-ray ... There is low radiation exposure. X-rays are monitored and regulated to provide the minimum amount of radiation exposure needed to produce the image. Most ...

  4. Chest X-Ray

    Medline Plus

    Full Text Available ... talk with you about chest radiography also known as chest x-rays. Chest x-rays are the ... treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray ...

  5. X-ray resonant magnetic reflectivity of stratified magnetic structures: Eigenwave formalism and application to a W/Fe/W trilayer

    International Nuclear Information System (INIS)

    Elzo, M.; Jal, E.; Bunau, O.; Grenier, S.; Joly, Y.; Ramos, A.Y.; Tolentino, H.C.N.; Tonnerre, J.M.; Jaouen, N.

    2012-01-01

    A formalism for the reflectivity of electromagnetic waves by magnetic materials is presented with an application. It is applied to retrieve the magnetic moment density along the depth of magnetic materials with arbitrary magnetic moment direction using matricial algebra, including roughness between layers. The reflectivity is derived following a classical description with Maxwell equations and a permittivity built from the quantum scattering amplitude. Approximations on the relative power of the Thomson scattering and the magnetic terms are trackable in order to evaluate the validity of the formalism case-by-case, from the optical light regime up to soft and hard X-rays. Eigenwaves are used throughout the whole formalism. In order to illustrate the methodology, we present an application to a W/Fe/W trilayer performed at the Fe L-edge, in the soft X-ray regime. - Highlights: → Magnetism at interfaces and in thin films is increasingly studied. → X-ray resonant magnetic reflectivity yields the in depth magnetization profile in thin films. → We present a formalism and methodology to study the data. → We illustrate the technique with an example.

  6. X-ray optics and X-ray microscopes: new challenges

    International Nuclear Information System (INIS)

    Susini, J.

    2004-01-01

    Soon after the discovery of X-rays in 1895 by W. Roentgen, it became rapidly clear that the methods traditionally used in the visible light regime, namely refraction, diffraction and reflection were difficult to apply for X-ray optics. The physical origins of these difficulties are closely linked to the very nature of interaction of X-rays with matter. The small deviation δ of the refractive index of condensed matter from unity makes it difficult to extend refraction-based optics from the optical spectral region to the X-ray region because the refraction angle is proportional to δ. Similarly it is very challenging to extend diffraction-based focusing techniques to X-rays because the diffraction angle scales inversely with wavelength. Finally, the use of reflection-based optics is also limited by the very small critical angle for total reflection. All those fundamental limitations prevented for almost one century, the development of X-ray microscopy whereas electron microscopy became a standard tool. In the past twenty years, interests for X-ray microscopy revived, mainly because of several major advances in X-ray sources and X-ray optics. X-ray microscopy techniques are now emerging as powerful and complementary tools for submicron investigations. Soft X-ray microscopes offer traditionally the possibility to form direct images of thick hydrated biological material in near-native environment, at a spatial resolution well beyond that achievable with visible light microscopy. Natural contrast is available in the soft X-ray region, in the so-called ''water-window'', due to the presence of absorption edges of the major constituents (C,N,O). Recent advances in manufacturing techniques have enlarged the accessible energy range of micro-focussing optics and offer new applications in a broad range of disciplines. X-ray microscopy in the 1 - 30 keV energy range is better suited for fluorescence to map trace elements, tomography for 3D imaging and micro-diffraction. The

  7. X-ray astronomy

    International Nuclear Information System (INIS)

    Giacconi, R.; Gursky, H.

    1974-01-01

    This text contains ten chapters and three appendices. Following an introduction, chapters two through five deal with observational techniques, mechanisms for the production of x rays in a cosmic setting, the x-ray sky and solar x-ray emission. Chapters six through ten include compact x-ray sources, supernova remnants, the interstellar medium, extragalactic x-ray sources and the cosmic x-ray background. Interactions of x rays with matter, units and conversion factors and a catalog of x-ray sources comprise the three appendices. (U.S.)

  8. Center for X-ray Optics, 1988

    International Nuclear Information System (INIS)

    1989-04-01

    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

  9. The changing source of X-ray reflection in the radio-intermediate Seyfert 1 galaxy III Zw 2

    Science.gov (United States)

    Gonzalez, A. G.; Waddell, S. G. H.; Gallo, L. C.

    2018-03-01

    We report on X-ray observations of the radio-intermediate, X-ray bright Seyfert 1 galaxy, III Zw 2, obtained with XMM-Newton, Suzaku, and Swift over the past 17 yr. The source brightness varies significantly over yearly time-scales, but more modestly over periods of days. Pointed observations with XMM-Newton in 2000 and Suzaku in 2011 show spectral differences despite comparable X-ray fluxes. The Suzaku spectra are consistent with a power-law continuum and a narrow Gaussian emission feature at ˜6.4 keV, whereas the earlier XMM-Newton spectrum requires a broader Gaussian profile and soft-excess below ˜2 keV. A potential interpretation is that the primary power-law emission, perhaps from a jet base, preferentially illuminates the inner accretion disc in 2000, but the distant torus in 2011. The interpretation could be consistent with the hypothesized precessing radio jet in III Zw 2 that may have originated from disc instabilities due to an ongoing merging event.

  10. Detection limit calculations for different total reflection techniques

    International Nuclear Information System (INIS)

    Sanchez, H.J.

    2000-01-01

    In this work, theoretical calculations of detection limits for different total-reflection techniques are presented.. Calculations include grazing incidence (TXRF) and gracing exit (GEXRF) conditions. These calculations are compared with detection limits obtained for conventional x-ray fluorescence (XRF). In order to compute detection limits the Shiraiwa and Fujino's model to calculate x-ray fluorescence intensities was used. This model made certain assumptions and approximations to achieve the calculations, specially in the case of the geometrical conditions of the sample, and the incident and takeoff beams. Nevertheless the calculated data of detection limits for conventional XRF and total-reflection XRF show a good agreement with previous results. The model proposed here allows to analyze the different sources of background and the influence of the excitation geometry, which contribute to the understanding of the physical processes involved in the XRF analysis by total reflection. Finally, a comparison between detection limits in total-reflection analysis at grazing incidence and at grazing exit is carried out. Here a good agreement with the theoretical predictions of the reversibility principle is found, showing that detection limits are similar for both techniques. (author)

  11. Measurement of characteristic to total spectrum ratio of tungsten X-ray spectra for the validation of the modified Tbc model

    International Nuclear Information System (INIS)

    Lopez G, A. H.; Costa, P. R.; Tomal, A.

    2014-08-01

    Primary X-ray spectra were measured in the range of 80 to 150 kV in order to validate a computer program based on a semiempirical model for X-ray spectra evaluation(tbc and mod). The ratio between the characteristic lines and total spectrum was considered for comparing the simulated results and experimental data. The raw spectra measured by the Cd Te detector were corrected by the detector efficiency, Compton effects and characteristic Cd and Te X-rays escape peaks, using a software specifically developed. The software Origin 8.5.1 was used to calculate the spectra and characteristic peaks areas. The obtained result shows that the experimental spectra have higher effective energy than the simulated spectra computed with tbc and mod software. The behavior of the ratio between the characteristic lines and total spectrum for simulated data presents discrepancy with the experimental result. Computed results are in good agreement with theoretical data published by Green, for spectra obtained with 3.04 mm of additional aluminum filtration. The difference of characteristic to total spectrum ratio between experimental and simulated data increases with the tube voltage. (Author)

  12. Measurement of characteristic to total spectrum ratio of tungsten X-ray spectra for the validation of the modified Tbc model

    Energy Technology Data Exchange (ETDEWEB)

    Lopez G, A. H.; Costa, P. R. [University of Sao Paulo, Institute of Physics, Laboratory of Radiation Dosimetry and Medical Physics, Matao Street, alley R, 187, 66318 Sao Paulo (Brazil); Tomal, A., E-mail: ahlopezg@usp.br [Universidade Federal de Goias, Physics Institute, Campus Samambaia, 131 Goiania, Goias (Brazil)

    2014-08-15

    Primary X-ray spectra were measured in the range of 80 to 150 kV in order to validate a computer program based on a semiempirical model for X-ray spectra evaluation(tbc and mod). The ratio between the characteristic lines and total spectrum was considered for comparing the simulated results and experimental data. The raw spectra measured by the Cd Te detector were corrected by the detector efficiency, Compton effects and characteristic Cd and Te X-rays escape peaks, using a software specifically developed. The software Origin 8.5.1 was used to calculate the spectra and characteristic peaks areas. The obtained result shows that the experimental spectra have higher effective energy than the simulated spectra computed with tbc and mod software. The behavior of the ratio between the characteristic lines and total spectrum for simulated data presents discrepancy with the experimental result. Computed results are in good agreement with theoretical data published by Green, for spectra obtained with 3.04 mm of additional aluminum filtration. The difference of characteristic to total spectrum ratio between experimental and simulated data increases with the tube voltage. (Author)

  13. Chest X-Ray

    Medline Plus

    Full Text Available ... about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed x-ray exams and use a very small dose of ... of the inside of the chest. A chest x-ray is used to evaluate the lungs, heart and ...

  14. X-ray data processing

    OpenAIRE

    Powell, Harold R.

    2017-01-01

    The method of molecular structure determination by X-ray crystallography is a little over a century old. The history is described briefly, along with developments in X-ray sources and detectors. The fundamental processes involved in measuring diffraction patterns on area detectors, i.e. autoindexing, refining crystal and detector parameters, integrating the reflections themselves and putting the resultant measurements on to a common scale are discussed, with particular reference to the most c...

  15. Resonant soft x-ray reflectivity of Me/B4C multilayers near the boron K edge

    Energy Technology Data Exchange (ETDEWEB)

    Ksenzov, Dmitriy; Schlemper, Christoph; Pietsch, Ullrich

    2010-09-01

    Energy dependence of the optical constants of boron carbide in the short period Ru/B4C and Mo/B4C multilayers (MLs) are evaluated from complete reflectivity scans across the boron K edge using the energy-resolved photon-in-photon-out method. Differences between the refractive indices of the B4Cmaterial inside and close to the surface are obtained from the peak profile of the first order ML Bragg peak and the reflection profile near the critical angle of total external reflection close to the surface. Where a Mo/B4C ML with narrow barrier layers appears as a homogeneous ML at all energies, a Ru/B4C ML exhibits another chemical nature of boron at the surface compared to the bulk. From evaluation of the critical angle of total external reflection in the energy range between 184 and 186 eV, we found an enriched concentration of metallic boron inside the Ru-rich layer at the surface, which is not visible in other energy ranges.

  16. X-ray sky

    International Nuclear Information System (INIS)

    Gruen, M.; Koubsky, P.

    1977-01-01

    The history is described of the discoveries of X-ray sources in the sky. The individual X-ray detectors are described in more detail, i.e., gas counters, scintillation detectors, semiconductor detectors, and the principles of X-ray spectrometry and of radiation collimation aimed at increased resolution are discussed. Currently, over 200 celestial X-ray sources are known. Some were identified as nebulae, in some pulsations were found or the source was identified as a binary star. X-ray bursts of novae were also observed. The X-ray radiation is briefly mentioned of spherical star clusters and of extragalactic X-ray sources. (Oy)

  17. Stress measurements by multi-reflection grazing-incidence X-ray diffraction method (MGIXD) using different radiation wavelengths and different incident angles

    International Nuclear Information System (INIS)

    Marciszko, Marianna; Baczmański, Andrzej; Braham, Chedly; Wróbel, Mirosław; Wroński, Sebastian; Cios, Grzegorz

    2017-01-01

    The presented study introduces the development of the multi-reflection grazing-incidence X-ray diffraction method (MGIXD) for residual stress determination. The proposed new methodology is aimed at obtaining more reliable experimental data and increasing the depth of non-destructive stress determination below the sample surface. To verify proposed method measurements were performed on a classical X-ray diffractometer (Cu Kα radiation) and using synchrotron radiation (three different wavelengths: λ = 1.2527 Å, λ = 1.5419 Å and λ = 1.7512 Å). The Al2017 alloy subjected to three different surface treatments was investigated in this study. The obtained results showed that the proposed development of MGIXD method, in which not only different incident angles but also different wavelengths of X-ray are used, can be successfully applied for residual stress determination, especially when stress gradients are present in the sample.

  18. X-ray fluorescence beamline at LNLS: components and some associated techniques

    International Nuclear Information System (INIS)

    Perez, CArlos A.; Radtke, Martin; Perez, Carlos; Tolentino, Helio; Vicentin, Flavio; Sanchez, Hector Jorge; Perez, Roberto D.

    1997-01-01

    Full text. In this work a general description of the Total Reflection X-Ray Fluorescence (TXRF) and the X-Ray Fluorescence Microprobe (XRFM) is presented. Components, equipment and experimental stations for the x-ray fluorescence beamline are described, regarding to the techniques mentioned above. Results from the simulations of a pair bended mirrors in a Kirkpatrick-Baez configuration, are shown. The simulations were performed with Shadow program. (author)

  19. Producing x-rays

    International Nuclear Information System (INIS)

    Mallozzi, P.J.; Epstein, H.M.; Jung, R.G.; Applebaum, D.C.; Fairand, B.P.; Gallagher, W.J.

    1977-01-01

    A method of producing x-rays by directing radiant energy from a laser onto a target is described. Conversion efficiency of at least about 3 percent is obtained by providing the radiant energy in a low-power precursor pulse of approximately uniform effective intensity focused onto the surface of the target for about 1 to 30 nanoseconds so as to generate an expanding unconfined coronal plasma having less than normal solid density throughout and comprising a low-density (underdense) region wherein the plasma frequency is less than the laser radiation frequency and a higher-density (overdense) region wherein the plasma frequency is greater than the laser radiation frequency and, about 1 to 30 nanoseconds after the precursor pulse strikes the target, a higher-power main pulse focused onto the plasma for about 10 -3 to 30 nanoseconds and having such power density and total energy that the radiant energy is absorbed in the underdense region and conducted into the overdense region to heat it and thus to produce x-rays therefrom with the plasma remaining substantially below normal solid density and thus facilitating the substantial emission of x-rays in the form of spectral lines arising from nonequilibrium ionization states

  20. Magnetic confinement, Alfven wave reflection, and the origins of X-ray and mass-loss 'dividing lines' for late-type giants and supergiants

    Science.gov (United States)

    Rosner, R.; An, C.-H.; Musielak, Z. E.; Moore, R. L.; Suess, S. T.

    1991-01-01

    A simple qualitative model for the origin of the coronal and mass-loss dividing lines separating late-type giants and supergiants with and without hot, X-ray-emitting corona, and with and without significant mass loss is discussed. The basic physical effects considered are the necessity of magnetic confinement for hot coronal material on the surface of such stars and the large reflection efficiency for Alfven waves in cool exponential atmospheres. The model assumes that the magnetic field geometry of these stars changes across the observed 'dividing lines' from being mostly closed on the high effective temperature side to being mostly open on the low effective temperature side.

  1. Chemical and structural composition study through transmission and reflection electron microscopy and X-ray microanalysis of damaged duramater cardiac valves

    International Nuclear Information System (INIS)

    Verginelli, G.; Didio, L.J.A.; Puig, L.B.; Allen, D.J.; Highinson, G.H.; Zerbini, E.J.

    1982-01-01

    Ten malfunctioning durameter aortic prosthesis, excised surgically after 44 to 54 months of implantation were studied through transmission and reflection electron microscopy and X-ray microanalysis. Duramater extracted at necropsy but not used for valve prosthesis and duramater aortic prosthesis not implanted in patients were used as controls. It was concluded that homologous duramater valves present subcellular changes following implantation, with degenerating and proliferating areas which could correspond either to normal adaptation or consequence of degeneration - rebuilding which begins with implantation; it is also emphazised the need for ultramicroscopic studies in evaluating biological tissues and establishing its applicability in cardiac surgery. (M.A.C.) [pt

  2. Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Morgan, D. V. [National Security Technologies LLC, Los Alamos, New Mexico 87544 (United States)

    2016-08-15

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.

  3. Characterization of high viscosity materials by total reflection x-ray fluorescence

    International Nuclear Information System (INIS)

    Custo, G.; Boeykens, S.; Vazquez, C.

    2000-01-01

    Gel are soft, solid or solid-like materials of two or more components, one of which is a liquid present in substantial amount. It consists of three-dimensional polymer network and solvent and is an important state of matter. Polymer is a long-chain molecule that is composed of a large number of repeating units of identical structure. These macromolecules assemblies recently developed have interesting properties, which depends of their structure. Their impurities change these physical properties. The great inconvenient of these systems is their high viscosity that difficult sample preparation and analysis by most common chemical techniques. The purpose of this work is to explore the applicability of the TRXRF for the multi-elemental and structural analysis of synthetic and natural aqueous gels (mean polymer molecular weight greater than 10 3 ). The polymers investigated are scleroglucan, polyacrilamide, polyoxyethylene and xhantan. (author)

  4. Biomonitoring in rivers by total-reflection x-ray fluorescence analysis in macrozoobenthos samples

    International Nuclear Information System (INIS)

    Miesbauer, H.; Koeck, G.; Fuereder, L.

    2000-01-01

    A widespread set of analytical methods is used to control the fate of toxic metals in aquatic ecosystems. However, monitoring of water and sediments by metal analysis is not sufficient because of fluctuating metal concentrations in the water and delayed responses of sediments. It also provides little information about metal bioavailability in aquatic ecosystems. Therefore, aquatic organisms are increasingly used for biomonitoring the actual metal load of aquatic biota. Aquatic insects, in particular, satisfy some important criteria established for bioindicators, thus being valuable biomonitoring organisms of metal contamination in freshwater ecosystems. The presented paper describes the investigation of the metal contents of several benthic insect species (e.g. caddisfly larvae) from an Austrian river by using TXRF. Due to it's high sensitivity TXRF allows multi-element analysis of very low metal concentrations even in single individuals of aquatic insect larvae. Our results confirm TXRF to be valuable tool in environmental analysis. (author)

  5. Biomonitoring in rivers by total-reflection x-ray fluorescence analysis in macrozoobenthos samples

    International Nuclear Information System (INIS)

    Miesbauer, H.; Koeck, G.; Fuereder, L.

    2000-01-01

    A widespread set of analytical methods is used to control the fate of toxic metals in aquatic ecosystems. However, monitoring of water and sediments by metal analysis is not sufficient because of fluctuating metal concentrations in the water and delayed responses of sediments. It also provides little information about metal bio-availability in aquatic ecosystems. Therefore, aquatic organisms are increasingly used for bio-monitoring the actual metal load of aquatic biota. Aquatic insects, in particular, satisfy some important criteria established for bio-indicators, thus being valuable bio-monitoring organisms of metal contamination in freshwater ecosystems. The presented paper describes the investigation of the metal contents of several benthic insect species (e.g. caddisfly larvae) from an Austrian river by using TXRF. Due to it's high sensitivity TXRF allows multi-element analysis of very low metal concentrations even in single individuals of aquatic insect larvae. Our results confirm TXRF to be valuable tool in environmental analysis. (author)

  6. Application of total reflection x-ray fluorescence spectrometry in the textile industry

    International Nuclear Information System (INIS)

    Dogan, M.; Soylak, M.; Elci, L.; Bohlen, A. von

    2002-01-01

    In the present study, the determination of arsenic, lead, cadmium, chromium, cobalt, copper, nickel, mercury and zinc in various cloth samples produced in Kayseri-Turkey was performed after extraction with artificial sweat solution and decomposition with nitric acid. TXRF is shown to be suitable for the determination of 7 trace elements, down to the 0.001 (cobalt) to 0.004 (copper) mg/kg level in textile extract except for mercury and cadmium. The extractable part of the toxic metal's by artificial sweat solution is relatively low. In a few extracts the concentration values of Pb and Ni have exceeded their critical values of 0.2 mg/kg for lead and 1.0 mg/kg for nickel given by Oeko-Tex and determined for babies cloths. In addition, it was observed that the element pattern of textile samples resembled 'finger print type', TXRF-spectra. This technique can also be used for the identification of textile sample in forensic investigation. (author)

  7. Fingerprinting analysis of non-crystalline pharmaceutical compounds using high energy X-rays and the total scattering pair distribution function

    Science.gov (United States)

    Davis, Timur D.

    2011-12-01

    In the development of new medicinal products, poor oral bioavailability, due to the low solubilities of many active pharmaceutical ingredients (APIs), is increasingly a barrier for treatments to be administered using tablet or capsule formulations and one of the main challenges facing the pharmaceutical industry. Non-crystalline phases such as the amorphous and nanostructured states can confer increased solubility to a drug, and therefore, have recently garnered a lot of interest from pharmaceutical researchers. However, little is known about local ordering in non-crystalline pharmaceuticals due to the lack of reliable experimental probes, hindering the clinical application of these compounds. The powerful tools of crystallography begin to lose their potency for structures on the nanoscale; conventional X-ray powder diffraction (XRPD) patterns become broad and featureless in these cases and are not useful for differentiating between different local molecular packing arrangements. In this thesis, we introduce the use of high energy X-rays coupled with total scattering pair distribution function (TSPDF) and fingerprinting analysis to investigate the local structures of non-crystalline pharmaceutical compounds. The high energy X-rays allow us to experimentally collect diffuse scattering intensities, which contain information about a sample's local ordering, in addition to the Bragg scattering available in conventional XRPD experiments, while the TSPDF allows us to view the intra- and inter-molecular correlations in real space. The goal of this study was to address some fundamental problems involving fingerprinting non-crystalline APIs using TSPDF in order to lay the groundwork for the proper use of the technique by the pharmaceutical community. We achieved this by developing the methodology as well as the exploring the scientific implications. On the methodology side, we introduced PDFGetX3, a new software program for calculating TSPDFs that simplifies the procedure

  8. Surface and interface strains studied by x-ray diffraction

    International Nuclear Information System (INIS)

    Akimoto, Koichi; Emoto, Takashi; Ichimiya, Ayahiko

    1998-01-01

    The authors have developed a technique of X-ray diffraction in order to measure strain fields near semiconductor surface and interface. The diffraction geometry is using the extremely asymmetric Bragg-case bulk reflection of a small incident angle to the surface and a large angle exiting from the surface. The incident angle of the X-rays is set near critical angle of total reflection by tuning X-ray energy of synchrotron radiation at the Photon Factory, Japan. For thermally grown-silicon oxide/Si(100) interface, the X-ray intensity of the silicon substrate 311 reflection has been measured. From comparison of the full width at half maxima (FWHM) of X-ray rocking curves of various thickness of silicon oxides, it has been revealed that silicon substrate lattice is highly strained in the thin (less than about 5 nm) silicon oxide/silicon system. In order to know the original silicon surface strain, the authors have also performed the same kind of measurements in the ultra-high vacuum chamber. A clean Si(111) 7x7 surface gives sharper X-ray diffraction peak than that of the native oxide/Si(111) system. From these measurements, it is concluded that the thin silicon oxide film itself gives strong strain fields to the silicon substrates, which may be the reason of the existence of the structural transition layer at the silicon oxide/Si interface

  9. Chest X-Ray

    Medline Plus

    Full Text Available ... some concerns about chest x-rays. However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a ... posted: How to Obtain and Share ...

  10. Chest X-Ray

    Medline Plus

    Full Text Available ... X-ray Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey Rubin, a radiologist ... about chest x-rays, visit Radiology Info dot org. Thank you for your time! Spotlight Recently posted: ...

  11. X-ray apparatus

    International Nuclear Information System (INIS)

    Sell, L.J.

    1981-01-01

    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

  12. X-ray - skeleton

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003381.htm X-ray - skeleton To use the sharing features on this ... Degenerative bone conditions Osteomyelitis Risks There is low radiation exposure. X-rays machines are set to provide the smallest ...

  13. Iron overload of human colon adenocarcinoma cells studied by synchrotron-based X-ray techniques

    NARCIS (Netherlands)

    Mihucz, Victor G.; Meirer, Florian; Polgári, Zsófia; Réti, Andrea; Pepponi, Giancarlo; Ingerle, Dieter; Szoboszlai, Norbert; Streli, Christina

    2016-01-01

    Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge

  14. A structural investigation into the compaction behavior of pharmaceutical composites using powder X-ray diffraction and total scattering analysis.

    Science.gov (United States)

    Moore, Michael D; Steinbach, Alison M; Buckner, Ira S; Wildfong, Peter L D

    2009-11-01

    To use advanced powder X-ray diffraction (PXRD) to characterize the structure of anhydrous theophylline following compaction, alone, and as part of a binary mixture with either alpha-lactose monohydrate or microcrystalline cellulose. Compacts formed from (1) pure theophylline and (2) each type of binary mixture were analyzed intact using PXRD. A novel mathematical technique was used to accurately separate multi-component diffraction patterns. The pair distribution function (PDF) of isolated theophylline diffraction data was employed to assess structural differences induced by consolidation and evaluated by principal components analysis (PCA). Changes induced in PXRD patterns by increasing compaction pressure were amplified by the PDF. Simulated data suggest PDF dampening is attributable to molecular deviations from average crystalline position. Samples compacted at different pressures were identified and differentiated using PCA. Samples compacted at common pressures exhibited similar inter-atomic correlations, where excipient concentration factored in the analyses involving lactose. Practical real-space structural analysis of PXRD data by PDF was accomplished for intact, compacted crystalline drug with and without excipient. PCA was used to compare multiple PDFs and successfully differentiated pattern changes consistent with compaction-induced disordering of theophylline as a single component and in the presence of another material.

  15. Compositional Evolution of Calcium Silicate Hydrate (C-S-H) Structures by Total X-Ray Scattering

    KAUST Repository

    Soyer-Uzun, Sezen

    2011-12-09

    High-energy X-ray diffraction was employed to study the structural characteristics of a set of C-S-H samples with 0.6 ≤ C/S a;circ 1.75. It has been observed that Si is tetrahedrally coordinated to O for all samples irrespective of chemical composition and the Ca-O coordination number gradually decreases from ∼7 to ∼6 with increasing C/S ratio. This suggests that the C-S-H structure evolves from a tobermorite-like structure into a jennite-like structure as a function of increasing C/S ratio as the interlayer space decreases from ∼1.3 to ∼1 nm. Evolution of these short- and medium-range order structural characteristics in the C-S-H system is associated with the alteration of the Ca-O layers and silicate depolymerization with increasing C/S. © 2011 The American Ceramic Society.

  16. Compositional Evolution of Calcium Silicate Hydrate (C-S-H) Structures by Total X-Ray Scattering

    KAUST Repository

    Soyer-Uzun, Sezen; Chae, Sejung Rosie; Benmore, Chris J.; Wenk, Hans-Rudolf; Monteiro, Paulo J. M.

    2011-01-01

    High-energy X-ray diffraction was employed to study the structural characteristics of a set of C-S-H samples with 0.6 ≤ C/S a;circ 1.75. It has been observed that Si is tetrahedrally coordinated to O for all samples irrespective of chemical composition and the Ca-O coordination number gradually decreases from ∼7 to ∼6 with increasing C/S ratio. This suggests that the C-S-H structure evolves from a tobermorite-like structure into a jennite-like structure as a function of increasing C/S ratio as the interlayer space decreases from ∼1.3 to ∼1 nm. Evolution of these short- and medium-range order structural characteristics in the C-S-H system is associated with the alteration of the Ca-O layers and silicate depolymerization with increasing C/S. © 2011 The American Ceramic Society.

  17. The nuclear pore density in rat liver cells upon regeneration and total body X-ray irradiation

    International Nuclear Information System (INIS)

    Kuz'mina, S.N.; Troitskaya, L.P.; Mirkhamidova, P.A.; Bul'dyaeva, T.V.; Zbarskij, I.B.; Grigor'ev, V.B.; Akademiya Meditsinskikh Nauk SSSR, Moscow. Inst. Virusologii)

    1979-01-01

    The nuclear pore density has been investigated in rat liver cells in the course of regeneration and X-ray irradiation. It has been found that the number of pore complexes (PC) per nuclear shell (NS) unit area in the liver cells is not constant. In an hour following whole-body irradiation of rats with a regenerating liver at the 1200 R dose the number of PC per 1 μm 2 of the nuclear shell area decreases by 5, 8 times as compared with the PC density in the regenerating liver cells of the irradiated rats, the PC degradation and structural rupture being observed. It has been established by means of the freezing-etching method which enables PC surfaces observation as for cytoplasma as well as for nucleoplasma that the PC peripheral granulas and the central granula consist of subparticles being approximately of the same size. The central granula forms a channel through which the material containing RNA passes from the nucleus to the cytoplasma. On the basis of the fact that the treatement by Triton X-100, disarranging the integrity of the NS membranous structure, preserves PC in relation to the fibrous layer as well as on the basis of the unequal nuclear pore state observed on the platinum-carbon replicas from nuclei splits it is supposed that PC can be formed in the nucleus and then in the course of repening ''built in'' PS

  18. Change in fat-free mass assessed by bioelectrical impedance, total body potassium and dual energy X-ray absorptiometry during prolonged weight loss

    DEFF Research Database (Denmark)

    Hendel, H W; Gotfredsen, A; Højgaard, L

    1996-01-01

    A total of 16 obese women (body mass index (BMI) 30-43 kg m(-2)) participated in a weight reduction study. Before and after a weight loss of 11.7 +/- 7.4 kg (mean +/- SD), body composition was assessed by dual energy X-ray absorptiometry (DXA), and total body potassium counting (TBK). These measu......A total of 16 obese women (body mass index (BMI) 30-43 kg m(-2)) participated in a weight reduction study. Before and after a weight loss of 11.7 +/- 7.4 kg (mean +/- SD), body composition was assessed by dual energy X-ray absorptiometry (DXA), and total body potassium counting (TBK......). These measurements were compared with bioimpedance analysis (BIA) by applying 11 predictive BIA equations published in the literature. Predictive equations for the present study population were developed, with the use of fat-free mass (FFM) as assessed by TBK and DXA as references in multiple regression analysis....... The results of the BIA equations varied widely; FFM was generally overestimated by BIA as compared with DXA and TBK before and after weight loss. During weight loss, the FFM did not change, as estimated by DXA (1.3 +/- 2.3 kg, p > 0.05) and TBK (0.9 +/- 2.9 kg, p > 0.05). The recorded change in impedance (R...

  19. Chest X-Ray

    Medline Plus

    Full Text Available ... I’d like to talk with you about chest radiography also known as chest x-rays. Chest x-rays are the most ... far outweighs any risk. For more information about chest x-rays, visit Radiology Info dot org. Thank you for your time! ...

  20. 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 ...

  1. X-ray spectrometry

    International Nuclear Information System (INIS)

    Markowicz, A.A.; Van Grieken, R.E.

    1986-01-01

    In the period under review, i.e, through 1984 and 1985, some 600 articles on XRS (X-ray spectrometry) were published; most of these have been scanned and the most fundamental ones are discussed. All references will refer to English-language articles, unless states otherwise. Also general books have appeared on quantitative EPXMA (electron-probe X-ray microanalysis) and analytical electron microscopy (AEM) as well as an extensive review on the application of XRS to trace analysis of environmental samples. In the period under review no radically new developments have been seen in XRS. However, significant improvements have been made. Gain in intensities has been achieved by more efficient excitation, higher reflectivity of dispersing media, and better geometry. Better understanding of the physical process of photon- and electron-specimen interactions led to complex but more accurate equations for correction of various interelement effects. Extensive use of micro- and minicomputers now enables fully automatic operation, including qualitative analysis. However, sample preparation and presentation still put a limit to further progress. Although some authors find XRS in the phase of stabilization or even stagnation, further gradual developments are expected, particularly toward more dedicated equipment, advanced automation, and image analysis systems. Ways are outlined in which XRS has been improved in the 2 last years by excitation, detection, instrumental, methodological, and theoretical advances. 340 references

  2. Flash X-ray

    International Nuclear Information System (INIS)

    Sato, Eiichi

    2003-01-01

    Generation of quasi-monochromatic X-ray by production of weakly ionized line plasma (flash X-ray), high-speed imaging by the X-ray and high-contrast imaging by the characteristic X-ray absorption are described. The equipment for the X-ray is consisted from the high-voltage power supply and condenser, turbo molecular pump, and plasma X-ray tube. The tube has a long linear anticathode to produce the line plasma and flash X-ray at 20 kA current at maximum. X-ray spectrum is measured by the imaging plate equipped in the computed radiography system after diffracted by a LiF single crystal bender. Cu anticathode generates sharp peaks of K X-ray series. The tissue images are presented for vertebra, rabbit ear and heart, and dog heart by X-ray fluoroscopy with Ce anticathode. Generation of K-orbit characteristic X-ray with extremely low bremsstrahung is to be attempted for medical use. (N.I.)

  3. Wide field x-ray telescopes: Detecting x-ray transients/afterglows related to GRBs

    International Nuclear Information System (INIS)

    Hudec, Rene; Pina, Ladislav; Inneman, Adolf; Gorenstein, Paul

    1998-01-01

    The recent discovery of X-ray afterglows of GRBs opens the possibility of analyses of GRBs by their X-ray detections. However, imaging X-ray telescopes in current use mostly have limited fields of view. Alternative X-ray optics geometries achieving very large fields of view have been theoretically suggested in the 70's but not constructed and used so far. We review the geometries and basic properties of the wide-field X-ray optical systems based on one- and two-dimensional lobster-eye geometry and suggest technologies for their development and construction. First results of the development of double replicated X-ray reflecting flats for use in one-dimensional X-ray optics of lobster-eye type are presented and discussed. The optimum strategy for locating GRBs upon their X-ray counterparts is also presented and discussed

  4. A NuSTAR Observation of the Reflection Spectrum of the Low-Mass X-Ray Binary 4U 1728-34

    Science.gov (United States)

    Sleator, Clio C.; Tomsick, John A.; King, Ashley L.; Miller, Jon M.; Boggs, Steven E.; Bachetti, Matteo; Barret, Didier; Chenevez, Jerome; Christensen, Finn E.; Craig, William W.; hide

    2016-01-01

    We report on a simultaneous NuSTAR and Swift observation of the neutron star low-mass X-ray binary 4U 1728-34. We identified and removed four Type I X-ray bursts during the observation in order to study the persistent emission. The continuum spectrum is hard and described well by a blackbody with kT=1.5 keV and a cutoff power law with Lambda = 1.5, and a cutoff temperature of 25 keV. Residuals between 6 and 8 keV provide strong evidence of a broad Fe K(alpha) line. By modeling the spectrum with a relativistically blurred reflection model, we find an upper limit for the inner disk radius of R(sub in) < or = 2R(sub ISCO). Consequently, we find that R(sub NS) < or = 23 km, assuming M = 1.4 Stellar Mass and a = 0.15. We also find an upper limit on the magnetic field of B < or =2 x 10(exp 8) G.

  5. Surface induced smectic order in ionic liquids - an X-ray reflectivity study of [C22C1im]+[NTf2].

    Science.gov (United States)

    Mars, Julian; Hou, Binyang; Weiss, Henning; Li, Hailong; Konovalov, Oleg; Festersen, Sven; Murphy, Bridget M; Rütt, Uta; Bier, Markus; Mezger, Markus

    2017-10-11

    Surface induced smectic order was found for the ionic liquid 1-methyl-3-docosylimidazolium bis(trifluoromethlysulfonyl)imide by X-ray reflectivity and grazing incidence scattering experiments. Near the free liquid surface, an ordered structure of alternating layers composed of polar and non-polar moieties is observed. This leads to an oscillatory interfacial profile perpendicular to the liquid surface with a periodicity of 3.7 nm. Small angle X-ray scattering and polarized light microscopy measurements suggest that the observed surface structure is related to fluctuations into a metastable liquid crystalline SmA 2 phase that was found by supercooling the bulk liquid. The observed surface ordering persists up to 157 °C, i.e. more than 88 K above the bulk melting temperature of 68.1 °C. Close to the bulk melting point, we find a thickness of the ordered layer of L = 30 nm. The dependency of L(τ) = Λ ln(τ/τ 1 ) vs. reduced temperature τ follows a logarithmic growth law. In agreement with theory, the pre-factor Λ is governed by the correlation length of the isotropic bulk phase.

  6. Correlation of measured neon soft X-ray pulses of the INTI plasma focus with the reflected shock phase at 12KV

    International Nuclear Information System (INIS)

    Roy, Federico A. Jr; Chong, Perk Lin; Saw, S.H.

    2014-01-01

    The six-phase Lee Model Code is used to fit the computed current waveform to the measured waveform of the INTI Plasma Focus (PF;2.2 kJ at 12 kV), a T2 PF device, operated as a source of Neon soft X-ray (SXR) with optimum yield around 2.5 - 3 Torr of neon. The characteristic He-like and H-like neon line SXR pulse is measured using a pair of SXR detectors with selected filters that, by subtraction, have a photon energy window of 900 to 1550 eV covering the region of the characteristic neon SXR lines. The aim of this paper is to investigate the correlation between the time histories of the measured Neon soft X-ray pulse and the reflected shock phase of the computed current waveform which has been fitted to the measured current waveform. Results shows that the characteristic neon SXR measured at 3.17 J with a pulse duration of 249 ns starts typically after the radial inward shock phase and increases in magnitude few ns before the pinch phase. It tails unto the first anomalous resistance, and decays at the second anomalous resistance. (author)

  7. X-ray supermirrors for BESSY II

    International Nuclear Information System (INIS)

    Erko, A.; Schaefers, F.; Vidal, B.; Yakshin, A.; Pietsch, U.; Mahler, W.

    1995-01-01

    X-ray multilayer supermirrors for the energy range up to 20 keV have been theoretically studied and experimentally measured with synchrotron radiation. A multilayer mirror with 50 W/Si bilayers with different thicknesses on the Si substrate has a smooth reflectivity of up to 32% in the whole energy range from 5 to 22 keV at a grazing incidence angle of 0.32 degree which is considerably larger than using total external reflection. copyright 1995 American Institute of Physics

  8. X-ray astronomy

    International Nuclear Information System (INIS)

    Culhane, J.L.; Sanford, P.W.

    1981-01-01

    X-ray astronomy has been established as a powerful means of observing matter in its most extreme form. The energy liberated by sources discovered in our Galaxy has confirmed that collapsed stars of great density, and with intense gravitational fields, can be studied by making observations in the X-ray part of the electromagnetic spectrum. The astronomical objects which emit detectable X-rays include our own Sun and extend to quasars at the edge of the Universe. This book describes the history, techniques and results obtained in the first twenty-five years of exploration. Space rockets and satellites are essential for carrying the instruments above the Earth's atmosphere where it becomes possible to view the X-rays from stars and nebulae. The subject is covered in chapters, entitled: the birth of X-ray astronomy; the nature of X-radiation; X-rays from the Sun; solar-flare X-rays; X-rays from beyond the solar system; supernovae and their remnants; X-rays from binary stars; white dwarfs and neutron stars; black holes; X-rays from galaxies and quasars; clusters of galaxies; the observatories of the future. (author)

  9. X-ray data processing.

    Science.gov (United States)

    Powell, Harold R

    2017-10-31

    The method of molecular structure determination by X-ray crystallography is a little over a century old. The history is described briefly, along with developments in X-ray sources and detectors. The fundamental processes involved in measuring diffraction patterns on area detectors, i.e. autoindexing, refining crystal and detector parameters, integrating the reflections themselves and putting the resultant measurements on to a common scale are discussed, with particular reference to the most commonly used software in the field. © 2017 The Author(s).

  10. Copper doped TiO2 nanoparticles characterized by X-ray absorption spectroscopy, total scattering, and powder diffraction--a benchmark structure-property study.

    Science.gov (United States)

    Lock, Nina; Jensen, Ellen M L; Mi, Jianli; Mamakhel, Aref; Norén, Katarina; Qingbo, Meng; Iversen, Bo B

    2013-07-14

    Metal functionalized nanoparticles potentially have improved properties e.g. in catalytic applications, but their precise structures are often very challenging to determine. Here we report a structural benchmark study based on tetragonal anatase TiO2 nanoparticles containing 0-2 wt% copper. The particles were synthesized by continuous flow synthesis under supercritical water-isopropanol conditions. Size determination using synchrotron PXRD, TEM, and X-ray total scattering reveals 5-7 nm monodisperse particles. The precise dopant structure and thermal stability of the highly crystalline powders were characterized by X-ray absorption spectroscopy and multi-temperature synchrotron PXRD (300-1000 K). The combined evidence reveals that copper is present as a dopant on the particle surfaces, most likely in an amorphous oxide or hydroxide shell. UV-VIS spectroscopy shows that copper presence at concentrations higher than 0.3 wt% lowers the band gap energy. The particles are unaffected by heating to 600 K, while growth and partial transformation to rutile TiO2 occur at higher temperatures. Anisotropic unit cell behavior of anatase is observed as a consequence of the particle growth (a decreases and c increases).

  11. Transmission X-ray mirror

    International Nuclear Information System (INIS)

    Lairson, B.M.; Bilderback, D.H.

    1982-01-01

    Transmission X-ray mirrors have been made from 400 A to 10 000 A thick soap films and have been shown to have novel properties. Using grazing angles of incidence, low energy X-rays were reflected from the front surface while more energetic X-rays were transmitted through the mirror largely unattenuated. A wide bandpass monochromator was made from a silicon carbide mirror followed by a soap film transmission mirror and operated in the white beam at the cornell High Energy Synchrotron Source (CHESS). Bandpasses of ΔE/E=12% to 18% were achieved at 13 keV with peak efficiencies estimated to be between 55% and 75%, respectively. Several wide angle scattering photographs of stretched polyethylene and a phospholipid were obtained in 10 s using an 18% bandpass. (orig.)

  12. Driving force behind adsorption-induced protein unfolding: a time-resolved X-ray reflectivity study on lysozyme adsorbed at an air/water interface.

    Science.gov (United States)

    Yano, Yohko F; Uruga, Tomoya; Tanida, Hajime; Toyokawa, Hidenori; Terada, Yasuko; Takagaki, Masafumi; Yamada, Hironari

    2009-01-06

    Time-resolved X-ray reflectivity measurements for lysozyme (LSZ) adsorbed at an air/water interface were performed to study the mechanism of adsorption-induced protein unfolding. The time dependence of the density profile at the air/water interface revealed that the molecular conformation changed significantly during adsorption. Taking into account previous work using Fourier transform infrared (FTIR) spectroscopy, we propose that the LSZ molecules initially adsorbed on the air/water interface have a flat unfolded structure, forming antiparallel beta-sheets as a result of hydrophobic interactions with the gas phase. In contrast, as adsorption continues, a second layer forms in which the molecules have a very loose structure having random coils as a result of hydrophilic interactions with the hydrophilic groups that protrude from the first layer.

  13. Quadrupole lamp furnace for high temperature (up to 2050 K) synchrotron powder x-ray diffraction studies in air in reflection geometry

    International Nuclear Information System (INIS)

    Sarin, P.; Yoon, W.; Jurkschat, K.; Zschack, P.; Kriven, W. M.

    2006-01-01

    A four-lamp thermal image furnace has been developed to conduct high temperature x-ray diffraction in reflection geometry on oxide ceramic powder samples in air at temperatures ≤2050 K using synchrotron radiation. A refractory crucible made of Pt20%Rh alloy was used as a specimen holder. A material with well characterized lattice expansion properties was used as an internal crystallographic thermometer to determine the specimen temperature and displacement. The performance of the apparatus was verified by measurement of the thermal expansion properties of CeO 2 , MgO, and Pt which were found to be within ±3% of the acceptable values. The advantages, limitations, and important considerations of the instrument developed are discussed

  14. X-ray holography

    International Nuclear Information System (INIS)

    Faigel, G.; Tegze, M.; Belakhovsky, M.; Marchesini, S.; Bortel, G.

    2003-01-01

    In the last decade holographic methods using hard X-rays were developed. They are able to resolve atomic distances, and can give the 3D arrangement of atoms around a selected element. Therefore, hard X-ray holography has potential applications in chemistry, biology and physics. In this article we give a general description of these methods and discuss the developments in the experimental technique. The capabilities of hard X-ray holography are demonstrated by examples

  15. Providing x-rays

    International Nuclear Information System (INIS)

    Mallozzi, P.J.; Epstein, H.M.

    1985-01-01

    This invention provides an apparatus for providing x-rays to an object that may be in an ordinary environment such as air at approximately atmospheric pressure. The apparatus comprises: means (typically a laser beam) for directing energy onto a target to produce x-rays of a selected spectrum and intensity at the target; a fluid-tight enclosure around the target; means for maintaining the pressure in the first enclosure substantially below atmospheric pressure; a fluid-tight second enclosure adjoining the first enclosure, the common wall portion having an opening large enough to permit x-rays to pass through but small enough to allow the pressure reducing means to evacuate gas from the first enclosure at least as fast as it enters through the opening; the second enclosure filled with a gas that is highly transparent to x-rays; the wall of the second enclosure to which the x-rays travel having a portion that is highly transparent to x-rays (usually a beryllium or plastic foil), so that the object to which the x-rays are to be provided may be located outside the second enclosure and adjacent thereto and thus receive the x-rays substantially unimpeded by air or other intervening matter. The apparatus is particularly suited to obtaining EXAFS (extended x-ray fine structure spectroscopy) data on a material

  16. Smart X-ray optics

    International Nuclear Information System (INIS)

    Michette, A G; Pfauntsch, S J; Sahraei, S; Shand, M; Morrison, G R; Hart, D; Vojnovic, B; Stevenson, T; Parkes, W; Dunare, C; Willingale, R; Feldman, C; Button, T; Zhang, D; Rodriguez-Sanmartin, D; Wang, H

    2009-01-01

    This paper describes reflective adaptive/active optics for applications including studies of biological radiation damage. The optics work on the polycapillary principle, but use arrays of channels in thin silicon. For optimum performance the x-rays should reflect once off a channel wall in each of two successive arrays. This reduces aberrations since then the Abbe sine condition is approximately satisfied. Adaptivity is achieved by flexing the arrays via piezo actuation, providing further aberration reduction and controllable focal length.

  17. Some simple ideas on x-ray reflection and grazing-incidence diffraction from thin surfactant films

    DEFF Research Database (Denmark)

    Kjær, K.

    1994-01-01

    For Langmuir films of long linear amphiphilic molecules at the air-water interface, grazing-incidence diffraction data resolved in terms of both the horizontal and vertical components of the scattering angle can be evaluated to a fair level of detail by means of a slide rule. Specular reflection ...... data require more sophisticated means although some rules of thumb can be formulated.......For Langmuir films of long linear amphiphilic molecules at the air-water interface, grazing-incidence diffraction data resolved in terms of both the horizontal and vertical components of the scattering angle can be evaluated to a fair level of detail by means of a slide rule. Specular reflection...

  18. Total L-shell X-ray production cross sections by 400-700 keV proton impact for elements with 34≤Z≤53

    International Nuclear Information System (INIS)

    Miranda, J.; Ledesma, R.; Lucio, O.G. de

    2001-01-01

    Total L-shell X-ray production cross sections induced by protons with energies between 400 and 700 keV were measured for elements with atomic number Z between 34 and 53. The ECPSSR theory describes appropriately the results. This model modifies the plane wave born approximation by considering projectile energy loss (E), Coulomb deflection of the incoming ion (C), polarization and change in electron binding energies through a perturbed stationary states method (PSS) and relativistic values of target electron mass (R). A comparison is given with previously published data for proton energies below 1 MeV and 26 ≤ Z ≤ 53, based on a scaling obtained from a reduced velocity parameter ξ L R . The results show that the scaling for these atomic numbers and energy ranges is adequate and a semi-empirical expression to calculate those cross sections is proposed

  19. Determination of the X-ray structure of the snake venom protein omwaprin by total chemical synthesis and racemic protein crystallography.

    Science.gov (United States)

    Banigan, James R; Mandal, Kalyaneswar; Sawaya, Michael R; Thammavongsa, Vilasak; Hendrickx, Antoni P A; Schneewind, Olaf; Yeates, Todd O; Kent, Stephen B H

    2010-10-01

    The 50-residue snake venom protein L-omwaprin and its enantiomer D-omwaprin were prepared by total chemical synthesis. Radial diffusion assays were performed against Bacillus megaterium and Bacillus anthracis; both L- and D-omwaprin showed antibacterial activity against B. megaterium. The native protein enantiomer, made of L-amino acids, failed to crystallize readily. However, when a racemic mixture containing equal amounts of L- and D-omwaprin was used, diffraction quality crystals were obtained. The racemic protein sample crystallized in the centrosymmetric space group P2(1)/c and its structure was determined at atomic resolution (1.33 A) by a combination of Patterson and direct methods based on the strong scattering from the sulfur atoms in the eight cysteine residues per protein. Racemic crystallography once again proved to be a valuable method for obtaining crystals of recalcitrant proteins and for determining high-resolution X-ray structures by direct methods.

  20. Accelerating an Ordered-Subset Low-Dose X-Ray Cone Beam Computed Tomography Image Reconstruction with a Power Factor and Total Variation Minimization.

    Science.gov (United States)

    Huang, Hsuan-Ming; Hsiao, Ing-Tsung

    2016-01-01

    In recent years, there has been increased interest in low-dose X-ray cone beam computed tomography (CBCT) in many fields, including dentistry, guided radiotherapy and small animal imaging. Despite reducing the radiation dose, low-dose CBCT has not gained widespread acceptance in routine clinical practice. In addition to performing more evaluation studies, developing a fast and high-quality reconstruction algorithm is required. In this work, we propose an iterative reconstruction method that accelerates ordered-subsets (OS) reconstruction using a power factor. Furthermore, we combine it with the total-variation (TV) minimization method. Both simulation and phantom studies were conducted to evaluate the performance of the proposed method. Results show that the proposed method can accelerate conventional OS methods, greatly increase the convergence speed in early iterations. Moreover, applying the TV minimization to the power acceleration scheme can further improve the image quality while preserving the fast convergence rate.

  1. Study of interface correlation in W/C multilayer structure by specular and non-specular grazing incidence X-ray reflectivity measurements

    Energy Technology Data Exchange (ETDEWEB)

    Biswas, A., E-mail: arupb@barc.gov.in; Bhattacharyya, D.; Sahoo, N. K. [Atomic and Molecular Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Maidul Haque, S.; Tripathi, S.; De, Rajnarayan [Atomic and Molecular Physics Division, Bhabha Atomic Research Centre, VIZAG Centre, Visakhapatnam 530012 (India); Rai, S. [Indus Synchrotron Utilization Division, Raja Raman Centre for Advanced Technology, Indore 452013 (India)

    2015-10-28

    W/C/W tri-layer thin film samples have been deposited on c-Si substrates in a home-built Ion Beam Sputtering system at 1.5 × 10{sup −3} Torr Ar working pressure and 10 mA grid current. The tri-layer samples have been deposited at different Ar{sup +} ion energies between 0.6 and 1.2 keV for W layer deposition and the samples have been characterized by specular and non-specular grazing incidence X-ray reflectivity (GIXR) measurements. By analyzing the GIXR spectra, various interface parameters have been obtained for both W-on-C and C-on-W interfaces and optimum Ar{sup +} ion energy for obtaining interfaces with low imperfections has been found. Subsequently, multilayer W/C samples with 5-layer, 7-layer, 9-layer, and 13-layer have been deposited at this optimum Ar{sup +} ion energy. By fitting the specular and diffused GIXR data of the multilayer samples with the parameters of each interface as fitting variables, different interface parameters, viz., interface width, in-plane correlation length, interface roughness, and interface diffusion have been estimated for each interface and their variation across the depth of the multilayers have been obtained. The information would be useful in realizing W/C multilayers for soft X-ray mirror application in the <100 Å wavelength regime. The applicability of the “restart of the growth at the interface” model in the case of these ion beam sputter deposited W/C multilayers has also been investigated in the course of this study.

  2. X-ray interferometers

    International Nuclear Information System (INIS)

    Franks, A.

    1980-01-01

    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.)

  3. Extremity x-ray

    Science.gov (United States)

    ... page: //medlineplus.gov/ency/article/003461.htm Extremity x-ray To use the sharing features on this page, ... in the body Risks There is low-level radiation exposure. X-rays are monitored and regulated to provide the ...

  4. X-rays utilization

    International Nuclear Information System (INIS)

    Rebigan, F.

    1979-03-01

    The modality of X-ray utilization in different activities and economy is given. One presents firstly quantities and units used in radiation dosimetry and other fields. One gives the generation of X-rays, their properties as well as the elements of radiation protection. The utilization characteristics of these radiations in different fields are finally given. (author)

  5. 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, ... d like to talk with you about chest radiography also known as chest x-rays. Chest x- ...

  6. Radiation therapy for angiosarcoma of the scalp: treatment outcomes of total scalp irradiation with X-rays and electrons.

    Science.gov (United States)

    Hata, Masaharu; Wada, Hidefumi; Ogino, Ichiro; Omura, Motoko; Koike, Izumi; Tayama, Yoshibumi; Odagiri, Kazumasa; Kasuya, Takeo; Inoue, Tomio

    2014-10-01

    Wide surgical excision is the standard treatment for angiosarcoma of the scalp, but many patients are inoperable. Therefore, we investigated the outcome of radiation therapy for angiosarcoma of the scalp. Seventeen patients with angiosarcoma of the scalp underwent radiation therapy with total scalp irradiation. Four patients had cervical lymph node metastases, but none had distant metastases. A median initial dose of 50 Gy in 25 fractions was delivered to the entire scalp. Subsequently, local radiation boost to the tumor sites achieved a median total dose of 70 Gy in 35 fractions. Fourteen of the 17 patients developed recurrences during the median follow-up period of 14 months after radiation therapy; 7 had recurrences in the scalp, including primary tumor progression in 2 patients and new disease in 5, and 12 patients developed distant metastases. The primary progression-free, scalp relapse-free, and distant metastasis-free rates were 86, 67, and 38 % at 1 year and 86, 38, and 16 % at 3 years, respectively. Thirteen patients died; the overall and cause-specific survival rates were both 73 % at 1 year and 23 and 44 % at 3 years, respectively. The median survival time was 16 months. There were no therapy-related toxicities ≥ grade 3. Total scalp irradiation is safe and effective for local tumor control, but a dose of ≤ 50 Gy in conventional fractions may be insufficient to eradicate microscopic tumors. For gross tumors, a total dose of 70 Gy, and > 70 Gy for tumors with deep invasion, is recommended.

  7. Constrained Total Generalized p-Variation Minimization for Few-View X-Ray Computed Tomography Image Reconstruction.

    Science.gov (United States)

    Zhang, Hanming; Wang, Linyuan; Yan, Bin; Li, Lei; Cai, Ailong; Hu, Guoen

    2016-01-01

    Total generalized variation (TGV)-based computed tomography (CT) image reconstruction, which utilizes high-order image derivatives, is superior to total variation-based methods in terms of the preservation of edge information and the suppression of unfavorable staircase effects. However, conventional TGV regularization employs l1-based form, which is not the most direct method for maximizing sparsity prior. In this study, we propose a total generalized p-variation (TGpV) regularization model to improve the sparsity exploitation of TGV and offer efficient solutions to few-view CT image reconstruction problems. To solve the nonconvex optimization problem of the TGpV minimization model, we then present an efficient iterative algorithm based on the alternating minimization of augmented Lagrangian function. All of the resulting subproblems decoupled by variable splitting admit explicit solutions by applying alternating minimization method and generalized p-shrinkage mapping. In addition, approximate solutions that can be easily performed and quickly calculated through fast Fourier transform are derived using the proximal point method to reduce the cost of inner subproblems. The accuracy and efficiency of the simulated and real data are qualitatively and quantitatively evaluated to validate the efficiency and feasibility of the proposed method. Overall, the proposed method exhibits reasonable performance and outperforms the original TGV-based method when applied to few-view problems.

  8. Prospects for supermirrors in hard x-ray spectroscopy

    DEFF Research Database (Denmark)

    Joensen, Karsten D.; Gorenstein, Paul; Christensen, Finn Erland

    1994-01-01

    . The measured x-ray reflectivities are well accounted for by the standard dynamical theories of multilayer reflection. Hard x ray applications that could benefit from x-ray supermirror coatings include focusing and imaging instrumentation for astrophysics, collimating and focusing devices for synchrotron...

  9. A NuSTAR observation of the reflection spectrum of the low-mass X-ray binary 4U 1728-34

    DEFF Research Database (Denmark)

    Sleator, Clio C.; Tomsick, John A.; King, Ashley L.

    2016-01-01

    We report on a simultaneous NuSTAR and Swift observation of the neutron star low-mass X-ray binary 4U 1728-34. We identified and removed four Type I X-ray bursts during the observation in order to study the persistent emission. The continuum spectrum is hard and described well by a blackbody with...

  10. Detection of Reflection Features in the Neutron Star Low-mass X-Ray Binary Serpens X-1 with NICER

    DEFF Research Database (Denmark)

    Ludlam, R. M.; Miller, J. M.; Arzoumanian, Z.

    2018-01-01

    We present Neutron Star Interior Composition Explorer (NICER) observations of the neutron star (NS) low-mass X-ray binary Serpens X-1 during the early mission phase in 2017. With the high spectral sensitivity and low-energy X-ray passband of NICER, we are able to detect the Fe L line complex in a...

  11. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    Science.gov (United States)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  12. Lifting the veil on the X-ray universe

    Science.gov (United States)

    1999-11-01

    ESA's X-ray Multi Mirror mission - XMM - is the second Cornerstone in ESA's Long Term Scientific Programme (*). This new X-ray space telescope promises even more discoveries. With the large collecting area of its mirrors and the high sensitivity of its cameras, XMM is expected to increase radically our understanding of high-energy sources - clues to a mysterious past, and keys to understanding the future of the Universe. 174 wafer-thin X-ray mirrors X-rays coming from celestial objects are highly energetic and elusive. They can best be measured and studied after focusing a sufficient number upon sensitive detectors. To achieve this, XMM's Mirror Modules have been given a gargantuan appetite for X-rays. The space observatory combines three barrel-shaped telescope modules. In each are nested 58 wafer-thin concentric mirror shells highly polished and subtly shaped. Passing through at an extremely shallow angle, the so-called "grazing incidence", the X-rays will be beamed to the science instruments situated on the focal plane at the other extremity of the satellite. The three mirror modules have a total mirror surface of over 120m2 - practically the size of a tennis court.. The collecting power of XMM's three telescopes is the greatest ever seen on an X-ray space mission, many times more than the most recently launched X-ray satellite. The design and assembly of the mirror modules, their testing for operation in space and their precise calibration constitute one of the greatest achievements of the XMM programme. The flimsy mirror shells, with their gold reflective surface on a nickel backing, were made by replication like carbon copies from master moulds. They were shaped to an accuracy of a thousandth of a millimetre, and then polished to a smoothness a thousand times better than that. Packaged one within another like Russian dolls, each mirror was focused and centred with respect to its neighbour to an accuracy of 25 microns - a quarter of the width of a human hair

  13. Radiation therapy for angiosarcoma of the scalp. Treatment outcomes of total scalp irradiation with X-rays and electrons

    Energy Technology Data Exchange (ETDEWEB)

    Hata, Masaharu; Koike, Izumi; Kasuya, Takeo; Inoue, Tomio [Yokohama City University Graduate School of Medicine, Department of Radiology, Yokohama, Kanagawa (Japan); Wada, Hidefumi [Yokohama City University Graduate School of Medicine, Department of Dermatology, Yokohama, Kanagawa (Japan); Ogino, Ichiro [Yokohama City University Medical Center, Department of Radiation Oncology, Yokohama, Kanagawa (Japan); Omura, Motoko [Yokohama City University Graduate School of Medicine, Department of Radiology, Yokohama, Kanagawa (Japan); Shonankamakura General Hospital, Department of Radiation Oncology, Kamakura, Kanagawa (Japan); Tayama, Yoshibumi [Yokohama Minami Kyousai Hospital, Department of Radiology, Yokohama, Kanagawa (Japan); Odagiri, Kazumasa [Yokohama City University Graduate School of Medicine, Department of Radiology, Yokohama, Kanagawa (Japan); Yokohama Municipal Citizen' s Hospital, Department of Radiation Oncology, Yokohama, Kanagawa (Japan)

    2014-10-15

    Wide surgical excision is the standard treatment for angiosarcoma of the scalp, but many patients are inoperable. Therefore, we investigated the outcome of radiation therapy for angiosarcoma of the scalp. Seventeen patients with angiosarcoma of the scalp underwent radiation therapy with total scalp irradiation. Four patients had cervical lymph node metastases, but none had distant metastases. A median initial dose of 50 Gy in 25 fractions was delivered to the entire scalp. Subsequently, local radiation boost to the tumor sites achieved a median total dose of 70 Gy in 35 fractions. Fourteen of the 17 patients developed recurrences during the median follow-up period of 14 months after radiation therapy; 7 had recurrences in the scalp, including primary tumor progression in 2 patients and new disease in 5, and 12 patients developed distant metastases. The primary progression-free, scalp relapse-free, and distant metastasis-free rates were 86, 67, and 38 % at 1 year and 86, 38, and 16 % at 3 years, respectively. Thirteen patients died; the overall and cause-specific survival rates were both 73 % at 1 year and 23 and 44 % at 3 years, respectively. The median survival time was 16 months. There were no therapy-related toxicities ≥ grade 3. Total scalp irradiation is safe and effective for local tumor control, but a dose of ≤ 50 Gy in conventional fractions may be insufficient to eradicate microscopic tumors. For gross tumors, a total dose of 70 Gy, and > 70 Gy for tumors with deep invasion, is recommended. (orig.) [German] Umfangreiche chirurgische Exzision ist die Standardbehandlung fuer Angiosarkome der Kopfhaut, aber viele Patienten sind nicht operierbar. Daher haben wir die Ergebnisse einer Strahlenbehandlung fuer Angiosarkome der Kopfhaut untersucht. Insgesamt 17 Patienten mit Angiosarkom der Kopfhaut erhielten eine Strahlenbehandlung der gesamten Kopfhaut. Vier Patienten hatten zervikale Lymphknotenmetastasen, aber keine Fernmetastasen. Die gesamte Kopfhaut

  14. Composition determination of quaternary GaAsPN layers from single X-ray diffraction measurement of quasi-forbidden (002) reflection

    Energy Technology Data Exchange (ETDEWEB)

    Tilli, J.-M., E-mail: juha-matti.tilli@iki.fi; Jussila, H.; Huhtio, T.; Sopanen, M. [Department of Micro and Nanosciences, Aalto University, P.O. Box 13500, FI-00076 Aalto (Finland); Yu, K. M. [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States)

    2014-05-28

    GaAsPN layers with a thickness of 30 nm were grown on GaP substrates with metalorganic vapor phase epitaxy to study the feasibility of a single X-ray diffraction (XRD) measurement for full composition determination of quaternary layer material. The method is based on the peak intensity of a quasi-forbidden (002) reflection, which is shown to vary with changing arsenic content for GaAsPN. The method works for thin films with a wide range of arsenic contents and shows a clear variation in the reflection intensity as a function of changing layer composition. The obtained thicknesses and compositions of the grown layers are compared with accurate reference values obtained by Rutherford backscattering spectroscopy combined with nuclear reaction analysis measurements. Based on the comparison, the error in the XRD defined material composition becomes larger with increasing nitrogen content and layer thickness. This suggests that the dominating error source is the deteriorated crystal quality due to the nonsubstitutional incorporation of nitrogen into the crystal lattice and strain relaxation. The results reveal that the method overestimates the arsenic and nitrogen content within error margins of about 0.12 and about 0.025, respectively.

  15. Total and Segmental Body Composition Examination in Collegiate Football Players Using Multifrequency Bioelectrical Impedance Analysis and Dual X-ray Absorptiometry.

    Science.gov (United States)

    Raymond, Christiana J; Dengel, Donald R; Bosch, Tyler A

    2018-03-01

    Raymond, CJ, Dengel, DR, and Bosch, TA. Total and segmental body composition examination in collegiate football players using multifrequency bioelectrical impedance analysis and dual X-ray absorptiometry. J Strength Cond Res 32(3): 772-782, 2018-The current study examined the influence of player position on the agreement between multifrequency bioelectrical impedance analysis (MfBIA) and dual X-ray absorptiometry (DXA) when assessing total and segmental percent body fat (BF%), fat mass (FM), and fat-free mass (FFM) in National Collegiate Athletic Association Division I collegiate football athletes. Forty-four male collegiate athletes (age = 19 ± 1 year; height = 1.9 ± 1.0 m; and body mass = 106.4 ± 18.8 kg) participated. Player positions included: offensive linemen (OL; n = 7), tight ends (TE; n = 4), wide receivers (WR; n = 9), defensive linemen (DL; n = 6), defensive backs (DB; n = 8), linebackers (LB; n = 6), and running backs (RB; n = 4). Total and segmental body composition measured using MfBIA were compared with values obtained using DXA. Compared with DXA, MfBIA underestimated BF% (3.0 ± 3.8%), total FM (2.5 ± 4.3 kg), arm FM (0.4 ± 0.8 kg), arm FFM (1.4 ± 0.9 kg), leg FM (2.8 ± 2.0 kg), and leg FFM (5.4 ± 2.4 kg) (all p FFM (-2.4 ± 4.5 kg) (p FFM), ±3.83 kg (leg FM), ±4.62 kg (leg FFM), and ±8.83 kg (total FFM). No significant differences were observed between devices for trunk FM (-0.3 ± 3.0 kg; p = 0.565) and trunk FFM (0.4 ± 2.4 kg; p = 0.278), with LOAs of ±5.92 and ±4.69 kg, respectively. Player position significantly affected all between-device mean body composition measurement differences (adjusted p ≤ 0.05), with OL demonstrating the greatest effect on each variable. Therefore, MfBIA does not seem accurate in examining between-player body composition in college football players.

  16. 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.

  17. Stellar X-Ray Polarimetry

    Science.gov (United States)

    Swank, J.

    2011-01-01

    Most of the stellar end-state black holes, pulsars, and white dwarfs that are X-ray sources should have polarized X-ray fluxes. The degree will depend on the relative contributions of the unresolved structures. Fluxes from accretion disks and accretion disk corona may be polarized by scattering. Beams and jets may have contributions of polarized emission in strong magnetic fields. The Gravity and Extreme Magnetism Small Explorer (GEMS) will study the effects on polarization of strong gravity of black holes and strong magnetism of neutron stars. Some part of the flux from compact stars accreting from companion stars has been reflected from the companion, its wind, or accretion streams. Polarization of this component is a potential tool for studying the structure of the gas in these binary systems. Polarization due to scattering can also be present in X-ray emission from white dwarf binaries and binary normal stars such as RS CVn stars and colliding wind sources like Eta Car. Normal late type stars may have polarized flux from coronal flares. But X-ray polarization sensitivity is not at the level needed for single early type stars.

  18. 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

  19. X-ray apparatus

    International Nuclear Information System (INIS)

    Bernstein, S.; Stagg, L.; Lambert, T.W.; Griswa, P.J.

    1976-01-01

    A patient support system for X-ray equipment in arteriographic studies of the heart is described in detail. The support system has been designed to overcome many of the practical problems encountered in using previous types of arteriographic X-ray equipment. The support system is capable of horizontal movement and, by a series of shafts attached to the main support system, the X-ray source and image intensifier or detector may be rotated through the same angle. The system is highly flexible and details are given of several possible operational modes. (U.K.)

  20. X-ray detector

    International Nuclear Information System (INIS)

    Whetten, N.R.; Houston, J.M.

    1977-01-01

    An ionization chamber for use in determining the spatial distribution of x-ray photons in tomography systems comprises a plurality of substantially parallel, planar anodes separated by parallel, planar cathodes and enclosed in a gas of high atomic weight at a pressure from approximately 10 atmospheres to approximately 50 atmospheres. The cathode and anode structures comprise metals which are substantially opaque to x-ray radiation and thereby tend to reduce the resolution limiting effects of x-ray fluoresence in the gas. In another embodiment of the invention the anodes comprise parallel conductive bars disposed between two planar cathodes. Guard rings eliminate surface leakage currents between adjacent electrodes. 8 figures

  1. X-ray apparatus

    International Nuclear Information System (INIS)

    Grady, J.K.

    1985-01-01

    X-ray apparatus is described which has a shutter between the X-ray source and the patient. The shutter controls the level of radiation to which the patient is exposed instead of merely discontinuing the electric power supplied to the source. When the shutter is opened a radiation sensor senses the level of X-radiation. When a preset quantity of X-radiation has been measured an exposure control closes the shutter. Instead of using the radiation sensor, the integrated power supplied to the anode of the X-ray source may be measured. (author)

  2. Bone X-Ray (Radiography)

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    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 ...

  3. Bone X-Ray (Radiography)

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    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 ...

  4. X-ray examination apparatus

    NARCIS (Netherlands)

    2000-01-01

    The invention relates to an X-ray apparatus which includes an adjustable X-ray filter. In order to adjust an intensity profile of the X-ray beam, an X-ray absorbing liquid is transported to filter elements of the X-ray filter. Such transport is susceptible to gravitational forces which lead to an

  5. Bone X-Ray (Radiography)

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    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 ...

  6. Bone X-Ray (Radiography)

    Science.gov (United States)

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

  7. Bone X-Ray (Radiography)

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

  8. 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 small ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  9. X-ray Observations at Gaisberg Tower

    Directory of Open Access Journals (Sweden)

    Pasan Hettiarachchi

    2018-01-01

    Full Text Available We report the occurrence of X-rays at ground level due to cloud-to-ground flashes of upward-initiated lightning from Gaisberg Tower, in Austria, which is located at an altitude of 1300 m. This is the first observation of X-ray emissions from upward lightning from a tower top located at high altitude. Measurements were carried out using scintillation detectors installed close to the tower top in two phases from 2011 to 2015. X-rays were recorded in three subsequent strokes of three flashes out of the total of 108 flashes recorded in the system during both phases. In contrast to the observations from downward natural or triggered lightning, X-rays were observed only within 10 µs before the subsequent return stroke. This shows that X-rays were emitted when the dart leader was in the vicinity of the tower top, hence during the most intense phase of the dart leader. Both the detected energy and the fluence of X-rays are far lower compared to X-rays from downward natural or rocket-triggered lightning. In addition to the above 108 flashes, an interesting observation of X-rays produced by a nearby downward flash is also presented. The shorter length of dart-leader channels in Gaisberg is suggested as a possible cause of this apparently weaker X-ray production.

  10. Chest X-Ray

    Medline Plus

    Full Text Available ... Disorders Video: The Basketball Game: An MRI Story Radiology and You Sponsored by Image/Video Gallery Your Radiologist Explains Chest X-ray Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey ...

  11. Chest X-Ray

    Medline Plus

    Full Text Available ... also be useful to help diagnose and monitor treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  12. X-ray tubes

    International Nuclear Information System (INIS)

    Young, R.W.

    1979-01-01

    A form of x-ray tube is described which provides satisfactory focussing of the electron beam when the beam extends for several feet from gun to target. Such a tube can be used for computerised tomographic scanning. (UK)

  13. Chest X-Ray

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    Full Text Available ... breath, persistent cough, fever, chest pain or injury. It may also be useful to help diagnose and ... have some concerns about chest x-rays. However, it’s important to consider the likelihood of benefit to ...

  14. Chest X-Ray

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    Full Text Available ... An MRI Story Radiology and You Sponsored by Image/Video Gallery Your Radiologist Explains Chest X-ray ... posted: How to Obtain and Share Your Medical Images Movement Disorders Video: The Basketball Game: An MRI ...

  15. Chest X-Ray

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    Full Text Available ... accurate diagnosis far outweighs any risk. For more information about chest x-rays, visit Radiology Info dot ... Inc. (RSNA). To help ensure current and accurate information, we do not permit copying but encourage linking ...

  16. Chest X-Ray

    Medline Plus

    Full Text Available ... Site Index A-Z Spotlight Recently posted: Pancreatic Cancer The Limitations of Online Dose Calculators Video: The ... of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  17. Chest X-Ray

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    Full Text Available ... exams and use a very small dose of ionizing radiation to produce pictures of the inside of the ... chest x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs ...

  18. 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. ...

  19. Chest X-Ray

    Medline Plus

    Full Text Available ... June is Men's Health Month Recently posted: Pancreatic Cancer The Limitations of Online Dose Calculators Video: The ... of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  20. X-ray metrology for ULSI structures

    International Nuclear Information System (INIS)

    Bowen, D. K.; Matney, K. M.; Wormington, M.

    1998-01-01

    Non-destructive X-ray metrological methods are discussed for application to both process development and process control of ULSI structures. X-ray methods can (a) detect the unacceptable levels of internal defects generated by RTA processes in large wafers, (b) accurately measure the thickness and roughness of layers between 1 and 1000 nm thick and (c) can monitor parameters such as crystallographic texture and the roughness of buried interfaces. In this paper we review transmission X-ray topography, thin film texture measurement, grazing-incidence X-ray reflectivity and high-resolution X-ray diffraction. We discuss in particular their suitability as on-line sensors for process control

  1. X-ray sources

    International Nuclear Information System (INIS)

    Masswig, I.

    1986-01-01

    The tkb market survey comparatively evaluates the X-ray sources and replacement tubes for stationary equipment currently available on the German market. It lists the equipment parameters of 235 commercially available X-ray sources and their replacement tubes and gives the criteria for purchase decisions. The survey has been completed with December 1985, and offers good information concerning medical and technical aspects as well as those of safety and maintenance. (orig.) [de

  2. Packing stress reduction in polymer-lipid monolayers at the air-water interface: An X-ray grazing-incidence diffraction and reflectivity study

    Energy Technology Data Exchange (ETDEWEB)

    Kuhl, T.L.; Majewski, J.; Howes, P.B.; Kjaer, K.; Nahmen, A. von; Lee, K.Y.C.; Ocko, B.; Israelachvili, J.N.; Smith, G.S.

    1999-08-25

    Using synchrotron grazing-incidence X-ray diffraction (GIXD) and reflectivity (XR), the authors have determined the in-plane and out-of-plane structure of phospholipid monolayers at the air-water interface as a function of hydrophilic lipid headgroup size. Di-stearoyl-phosphatidyl-ethanolamine (DSPE) lipid monolayers were systematically modified by chemically grafting hydrophilic poly(ethylene glycol) (PEG) chains of MW = 90 g/mol (2 ethylene oxide, EO, units), MW = 350 g/mol (8 EO units), and MW = 750 g/mol (17 EO units) to the lipid headgroups. The monolayers were studied in the solid phase at a surface pressure of 42 mN/m. At these high lipid packing densities, the PEG chains are submerged in the water subphase. The increased packing stresses from these bulky polymer headgroups distort the unit cell and the in-plane packing modes of the monolayers, leading to large out-of-plane alterations and staggering of the lipid molecules. Surprisingly, a change in the molecular packing of the monolayer toward higher packing densities (lower area per molecule) was observed on increasing the PEG MW to 750 g/mol (17 EO units). This rearrangement of the monolayer structure may be due to a conformational change in the PEG chains.

  3. A submicron synchrotron X-ray beam generated by capillary optics

    International Nuclear Information System (INIS)

    Engstroem, P.; Larsson, S.; Rindby, A.; Buttkewitz, A.; Garbe, S.; Gaul, G.; Knoechel, A.; Lechtenberg, F.; Deutsches Elektronen-Synchrotron

    1991-01-01

    A novel capillary optics technique for focusing synchrotron X-ray beams has been applied in an experiment performed at the DORIS storage ring at HASYLAB. This new technqiue, which utilizes the total reflection properties of X-rays inside small capillaries, has recently been applied to generate microbeams of X-rays, with a beam size down to about 10 μm using conventional X-ray tubes. The result from our recent experiment shows that capillary optics can also be used to generate a submicron beam of X-rays from a synchrotron light source. A description of the capillary unit, and the alignment procedure is given. The influence of the thermal load on the device caused by the intense flux of synchrotron radiation will be discussed. Future perspectives of the capillary techniques as applied to synchrotron radiation will be discussed. (orig.)

  4. Guiding hard x rays with glass polycapillary fiber

    International Nuclear Information System (INIS)

    Xiao, Q.F.; Ponomarev, I.Y.; Kolomitsev, A.I.; Gibson, D.M.; Dilmanian, F.A.; Nachaliel, E.

    1993-01-01

    X rays can be guided through a polycapillary fiber by multiple total reflections from the smooth channel walls of the fiber. Using monochromatic Synchrotron Radiation at energies of 22 and 44 keV, we measured the efficiency of transmission of x rays through polycapillary fibers with channel diameters of about 13 μm. Efficiencies of 57.3% and 54.5% for 22 keV and 44 keV x rays, respectively, were obtained with a 120-mm-long straight polycapillary fiber aligned with the incident beam. These values are close to the open fraction of the fiber, which is about 60%. In addition, transmission efficiency was measured as a function of the tilt angle between the incident beam and the axis of the fiber. We also measured the transmission efficiency as a function of the deflection angle for a 114-mm-long curved polycapillary fiber. The measurements are compared with a ray-tracing simulation

  5. Optical systems for synchrotron radiation: lecture 4. Soft x-ray imaging systems

    International Nuclear Information System (INIS)

    Howells, M.R.

    1986-04-01

    The history and present techniques of soft x-ray imaging are reviewed briefly. The physics of x-ray imaging is described, including the temporal and spatial coherence of x-ray sources. Particular technologies described are: contact x-ray microscopy, zone plate imaging, scanned image zone plate microscopy, scanned image reflection microscopy, and soft x-ray holography and diffraction

  6. Bone X-Ray (Radiography)

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    Full Text Available ... of knee x-rays. A portable x-ray machine is a compact apparatus that can be taken ... of the body being examined, an x-ray machine produces a small burst of radiation that passes ...

  7. Bone X-Ray (Radiography)

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    Full Text Available ... that might interfere with the x-ray images. Women should always inform their physician and x-ray ... Safety page for more information about radiation dose. Women should always inform their physician or x-ray ...

  8. Bone X-Ray (Radiography)

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    Full Text Available ... ray examination. X-rays usually have no side effects in the typical diagnostic range for this exam. ... x-rays. A Word About Minimizing Radiation Exposure Special care is taken during x-ray examinations to ...

  9. Bone X-Ray (Radiography)

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    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 ...

  10. Bone X-Ray (Radiography)

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    Full Text Available ... are the limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray ( ... leg (shin), ankle or foot. top of page What are some common uses of the procedure? A ...

  11. Bone X-Ray (Radiography)

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    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ...

  12. A new Mumford-Shah total variation minimization based model for sparse-view x-ray computed tomography image reconstruction.

    Science.gov (United States)

    Chen, Bo; Bian, Zhaoying; Zhou, Xiaohui; Chen, Wensheng; Ma, Jianhua; Liang, Zhengrong

    2018-04-12

    Total variation (TV) minimization for the sparse-view x-ray computer tomography (CT) reconstruction has been widely explored to reduce radiation dose. However, due to the piecewise constant assumption for the TV model, the reconstructed images often suffer from over-smoothness on the image edges. To mitigate this drawback of TV minimization, we present a Mumford-Shah total variation (MSTV) minimization algorithm in this paper. The presented MSTV model is derived by integrating TV minimization and Mumford-Shah segmentation. Subsequently, a penalized weighted least-squares (PWLS) scheme with MSTV is developed for the sparse-view CT reconstruction. For simplicity, the proposed algorithm is named as 'PWLS-MSTV.' To evaluate the performance of the present PWLS-MSTV algorithm, both qualitative and quantitative studies were conducted by using a digital XCAT phantom and a physical phantom. Experimental results show that the present PWLS-MSTV algorithm has noticeable gains over the existing algorithms in terms of noise reduction, contrast-to-ratio measure and edge-preservation.

  13. The potential for portable X-ray fluorescence determination of soil copper at ancient metallurgy sites, and considerations beyond measurements of total concentrations.

    Science.gov (United States)

    Tighe, M; Rogan, G; Wilson, S C; Grave, P; Kealhofer, L; Yukongdi, P

    2018-01-15

    Copper (Cu) at ancient metallurgy sites represents the earliest instance of anthropogenically generated metal pollution. Such sites are spread across a wide range of environments from Eurasia to South America, and provide a unique opportunity to investigate the past and present extent and impact of metalworking contamination. Establishing the concentration and extent of soil Cu at archaeometallurgy sites can enhance archaeological interpretations of site use but can also, more fundamentally, provide an initial indication of contamination risk from such sites. Systematic evaluations of total soil Cu concentrations at ancient metalworking sites have not been conducted, due in part to the limitations of conventional laboratory-based protocols. In this paper, we first review what is known about Cu soil concentrations at ancient metallurgy sites. We then assess the benefits and challenges of portable X-ray fluorescence spectrometry (pXRF) as an alternative, rapid technique for the assessment of background and contaminant levels of Cu in soils. We conclude that pXRF is an effective tool for identifying potential contamination. Finally, we provide an overview of some major considerations beyond total Cu concentrations, such as bioavailability assessments, that will need to be considered at such sites to move toward a complete assessment of environmental and human risk. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Discovery and development of x-ray diffraction

    Science.gov (United States)

    Jeong, Yeuncheol; Yin, Ming; Datta, Timir

    2013-03-01

    In 1912 Max Laue at University of Munich reasoned x-rays to be short wavelength electromagnetic waves and figured interference would occur when scattered off crystals. Arnold Sommerfeld, W. Wien, Ewald and others, raised objections to Laue's idea, but soon Walter Friedrich succeeded in recording x-ray interference patterns off copper sulfate crystals. But the Laue-Ewald's 3-dimensional formula predicted excess spots. Fewer spots were observed. William Lawrence Bragg then 22 year old studying at Cambridge University heard the Munich results from father William Henry Brag, physics professor at Univ of Leeds. Lawrence figured the spots are 2-d interference of x-ray wavelets reflecting off successive atomic planes and derived a simple eponymous equation, the Bragg equation d*sin(theta) = n*lamda. 1913 onward the Braggs dominated the crystallography. Max Laue was awarded the physics Nobel in 1914 and the Braggs shared the same in 1915. Starting with Rontgen's first ever prize in 1901, the importance of x-ray techniques is evident from the four out of a total 16 physics Nobels between 1901-1917. We will outline the historical back ground and importance of x-ray diffraction giving rise to techniques that even in 2013, remain work horses in laboratories all over the globe.

  15. Hard X-ray total scattering study on the structure of Si-dopped ferric oxyhydroxides and products of their transformation

    Science.gov (United States)

    Pieczara, Gabriela; Borkiewicz, Olaf; Manecki, Maciej; Rzepa, Grzegorz

    2016-04-01

    Here we report the results of a detailed structural investigation, using synchrotron-based pair distribution function analyses (PDF) and high-resolution X-ray diffraction (HR-XRD), on a series of Si-bearing synthetic analogues of ferrihydrite with a range of Si/Fe ratio relevant to geological environments and on products of their thermal transformation. Hard X-ray total scattering data suitable for PDF analyses have been collected at the PDF-dedicated beamline 11-ID-B and the HR-XRD data at beamline 11-BM of the Advanced Photon Source (APS) at Argonne National Laboratory (ANL). Ferrihydrite is a poorly crystalline, nano-sized hydrous ferric oxyhydroxide with a nominal/ideal formula Fe5HO8•4H2O. Its chemical composition however, can vary significantly and the atomic structure is yet to be fully understood despite multitude of structural studies undertaken over the past two decades (Michel et al., 2007; Manceau, 2009). One of the most commonly discussed and still unsettled contention points regarding the structural arrangements of ferrihydrite is related to the presence or absence of tetraherdally coordinated iron(III) within its structure. The majority of experimental work carried out to date focused on pure, synthetic ferrihydrite analogues with chemical composition close to ideal/nominal. This approach is clearly a significant oversimplification of natural ferrihydrite which always contains substantial amounts of admixtures, with Si, C, P, As, Ca, S and Al being the most common. One of the most important and the most commonly encountered impurities is Si, in the form of silicate ion that has strong affinity for ferrihydrite. SiO2content in natural ferrihydrites can vary substantially but generally falls with the range of 2.6-31.5 wt% (Cismasu et al., 2011). In certain environments however, such as modern seafloor hydrothermal vents, higher Si/Fe ratios (up to ca. 3) have been reported (Sun et al., 2013). The results of previous reports indicate that silicate

  16. Characterization of changes in total body composition for patients with head and neck cancer undergoing chemoradiotherapy using dual-energy x-ray absorptiometry.

    Science.gov (United States)

    Jackson, William; Alexander, Neil; Schipper, Matthew; Fig, Lorraine; Feng, Felix; Jolly, Shruti

    2014-09-01

    Patients with head and neck cancer experience significant weight loss secondary to concurrent chemoradiotherapy (CCRT). Using dual-energy X-ray absorptiometry (DEXA) scans, we characterize total body composition changes during and after CCRT in order to develop novel clinical care models that will improve the patient's quality of life (QOL). Sixty DEXA scans were obtained from 12 patients undergoing CCRT for locally advanced squamous cell head and neck cancer. DEXAs were performed at baseline, during treatment, completion of CCRT, and then 1 and 2 months posttreatment. Mean weight loss by treatment end was 9.5 kg (10.2%; p = .0002). On average, lean body mass (LBM) decreased 10.2% (p = .001), and fat body mass (FBM) decreased 11.1% (p = .001) during CCRT. LBM began to normalize after completion of treatment, whereas FBM continued to decline. Substantial loss of muscle and FBM occurs in patients undergoing CCRT for head and neck cancer. To prevent long-term disability and QOL decline after curative CCRT, clinical care interventions incorporating aggressive nutrition/exercise counseling are needed. Copyright © 2013 Wiley Periodicals, Inc.

  17. Timing the total reflection of light

    International Nuclear Information System (INIS)

    Chauvat, Dominique; Bonnet, Christophe; Dunseath, Kevin; Emile, Olivier; Le Floch, Albert

    2005-01-01

    We have identified for the first time the absolute delay at total reflection, envisioned by Newton. We show that there are in fact two divergent Wigner delays, depending on the polarisation of the incident light. These measurements give a new insight on the passage from total reflection to refraction

  18. X-Ray Absorption with Transmission X-Ray Microscopes

    NARCIS (Netherlands)

    de Groot, F.M.F.

    2016-01-01

    In this section we focus on the use of transmission X-ray microscopy (TXM) to measure the XAS spectra. In the last decade a range of soft X-ray and hard X-ray TXM microscopes have been developed, allowing the measurement of XAS spectra with 10–100 nm resolution. In the hard X-ray range the TXM

  19. Theoretical concepts of X-ray nanoscale analysis theory and applications

    CERN Document Server

    Benediktovitch, Andrei; Ulyanenkov, Alexander

    2013-01-01

    This book provides a concise survey of modern theoretical concepts of X-ray materials analysis. The principle features of the book are: basics of X-ray scattering, interaction between X-rays and matter and new theoretical concepts of X-ray scattering. The various X-ray techniques are considered in detail: high-resolution X-ray diffraction, X-ray reflectivity, grazing-incidence small-angle X-ray scattering and X-ray residual stress analysis. All the theoretical methods presented use the unified physical approach. This makes the book especially useful for readers learning and performing data ana

  20. Watching Nanoparticles Form: An In Situ (Small-/Wide-Angle X-ray Scattering/Total Scattering) Study of the Growth of Yttria-Stabilised Zirconia in Supercritical Fluids

    DEFF Research Database (Denmark)

    Tyrsted, Christoffer; Pauw, Brian; Jensen, Kirsten Marie Ørnsbjerg

    2012-01-01

    Understanding nanoparticle formation reactions requires multitechnique in situ characterisation, since no single characterisation technique provides adequate information. Here, the first combined small-angle X-ray scattering (SAXS)/wide-angle X-ray scattering (WAXS)/total-scattering study of nano...... of nanoparticle formation is presented. We report on the formation and growth of yttria-stabilised zirconia (YSZ) under the extreme conditions of supercritical methanol for particles with Y2O3 equivalent molar fractions of 0, 4, 8, 12 and 25%....