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Sample records for x-ray fluorescence atomic

  1. X-ray fluorescence experiment

    NASA Technical Reports Server (NTRS)

    Adler, I.; Trombka, J. I.; Gerard, J.; Schmadebeck, R.; Lowman, P.; Blodgett, H.; Yin, L.; Eller, E.; Lamothe, R.; Gorenstein, P.

    1972-01-01

    The preliminary results from the Sco X-1 and Cyg X-1 obtained from the Apollo 15 X-ray detector data are presented along with preliminary results of the X-ray fluorescence spectrometric data of the lunar surface composition. The production of the characteristic X-rays following the interaction of solar X-rays with the lunar surface is described along with the X-ray spectrometer. Preliminary analyses of the astronomical X-ray observation and the X-ray fluorescence data are presented.

  2. New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

    SciTech Connect

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.; Lanzirotti, A.; Newville, M.; Proslier, T.; Stodolna, J.; Sutton, S.; Tyliszczak, T.; Westphal, A.J.; Zasadzinski, J.

    2012-03-13

    Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution

  3. Atomic layer deposition to prevent metal transfer from implants: An X-ray fluorescence study

    NASA Astrophysics Data System (ADS)

    Bilo, Fabjola; Borgese, Laura; Prost, Josef; Rauwolf, Mirjam; Turyanskaya, Anna; Wobrauschek, Peter; Kregsamer, Peter; Streli, Christina; Pazzaglia, Ugo; Depero, Laura E.

    2015-12-01

    We show that Atomic Layer Deposition is a suitable coating technique to prevent metal diffusion from medical implants. The metal distribution in animal bone tissue with inserted bare and coated Co-Cr alloys was evaluated by means of micro X-ray fluorescence mapping. In the uncoated implant, the migration of Co and Cr particles from the bare alloy in the biological tissues is observed just after one month and the number of particles significantly increases after two months. In contrast, no metal diffusion was detected in the implant coated with TiO2. Instead, a gradient distribution of the metals was found, from the alloy surface going into the tissue. No significant change was detected after two months of aging. As expected, the thicker is the TiO2 layer, the lower is the metal migration.

  4. Fluorescence detection of white-beam X-ray absorption anisotropy: towards element-sensitive projections of local atomic structure

    PubMed Central

    Korecki, P.; Tolkiehn, M.; Dąbrowski, K. M.; Novikov, D. V.

    2011-01-01

    Projections of the atomic structure around Nb atoms in a LiNbO3 single crystal were obtained from a white-beam X-ray absorption anisotropy (XAA) pattern detected using Nb K fluorescence. This kind of anisotropy results from the interference of X-rays inside a sample and, owing to the short coherence length of a white beam, is visible only at small angles around interatomic directions. Consequently, the main features of the recorded XAA corresponded to distorted real-space projections of dense-packed atomic planes and atomic rows. A quantitative analysis of XAA was carried out using a wavelet transform and allowed well resolved projections of Nb atoms to be obtained up to distances of 10 Å. The signal of nearest O atoms was detected indirectly by a comparison with model calculations. The measurement of white-beam XAA using characteristic radiation indicates the possibility of obtaining element-sensitive projections of the local atomic structure in more complex samples. PMID:21997909

  5. Student X-Ray Fluorescence Experiments

    ERIC Educational Resources Information Center

    Fetzer, Homer D.; And Others

    1975-01-01

    Describes the experimental arrangement for x-ray analysis of samples which involves the following: the radioisotopic x-ray disk source; a student-built fluorescence chamber; the energy dispersive x-ray detector, linear amplifier and bias supply; and a multichannel pulse height analyzer. (GS)

  6. Nondestructive Characterization of Atomic Profiles in Layer-Structured Photovoltaic Materials Using the Method of Angular Dependence of X-Ray Fluorescence (ADXRF)

    SciTech Connect

    Kim, S.; Soo, Y. L.; Kioseoglou, G.; Huang, S.; Kao, Y. H.; Ramanathan, K.; Deb, S.

    2000-01-01

    Angular dependence of x-ray fluorescence technique has been applied to the study of atomic density profile in composite systems. This method is shown to be useful for probing the microstructures and intermixing of constituent elements in layer-structured photovoltaic materials.

  7. Apollo 15 X-ray fluorescence experiment

    NASA Technical Reports Server (NTRS)

    Adler, I.; Trombka, J.; Gerard, J.; Schmadebeck, R.; Lowman, P.; Blodgett, H.; Yin, L.; Eller, E.; Lamothe, R.; Gorenstein, P.

    1971-01-01

    The X-ray fluorescence spectrometer, carried in the SIM bay of the command service module was employed principally for compositional mapping of the lunar surface while in lunar orbit, and secondarily, for X-ray astronomical observations during the trans-earth coast. The lunar surface measurements involved observations of the intensity and characteristics energy distribution of the secondary or fluorescent X-rays produced by the interaction of solar X-rays with the lunar surface. The astronomical observations consisted of relatively long periods of measurements of X-rays from pre-selected galactic sources such as Cyg-X-1 and Sco X-1 as well as from the galactic poles.

  8. In situ synchrotron based x-ray fluorescence and scattering measurements during atomic layer deposition: Initial growth of HfO2 on Si and Ge substrates

    NASA Astrophysics Data System (ADS)

    Devloo-Casier, K.; Dendooven, J.; Ludwig, K. F.; Lekens, G.; D'Haen, J.; Detavernier, C.

    2011-06-01

    The initial growth of HfO2 was studied by means of synchrotron based in situ x-ray fluorescence (XRF) and grazing incidence small angle x-ray scattering (GISAXS). HfO2 was deposited by atomic layer deposition (ALD) using tetrakis(ethylmethylamino)hafnium and H2O on both oxidized and H-terminated Si and Ge surfaces. XRF quantifies the amount of deposited material during each ALD cycle and shows an inhibition period on H-terminated substrates. No inhibition period is observed on oxidized substrates. The evolution of film roughness was monitored using GISAXS. A correlation is found between the inhibition period and the onset of surface roughness.

  9. Atomic Data in X-Ray Astrophysics

    NASA Technical Reports Server (NTRS)

    Brickhouse, N. S.

    2000-01-01

    With the launches of the Chandra X-ray Observatory (CXO) and the X-ray Multimirror Mission (XMM) and the upcoming launch of the Japanese mission ASTRO-E, high resolution X-ray spectroscopy of cosmic sources has begun. Early, deep observations of three stellar coronal sources will provide not only invaluable calibration data, but will also give us benchmarks for the atomic data under collisional equilibrium conditions. Analysis of the Chandra X-ray Observatory data, and data from other telescopes taken simultaneously, for these stars is ongoing as part of the Emission Line Project. Goals of the Emission Line Project are: (1) to determine and verify accurate and robust diagnostics and (2) to identify and prioritize issues in fundamental spectroscopy which will require further theoretical and/or laboratory work. The Astrophysical Plasma Emission Database will be described in some detail, as it is introducing standardization and flexibility into X-ray spectral modeling. Spectral models of X-ray astrophysical plasmas can be generally classified as dominated by either collisional ionization or by X-ray photoionization. While the atomic data needs for spectral models under these two types of ionization are significantly different, there axe overlapping data needs, as I will describe. Early results from the Emission Line Project benchmarks are providing an invaluable starting place, but continuing work to improve the accuracy and completeness of atomic data is needed. Additionally, we consider the possibility that some sources will require that both collisional ionization and photoionization be taken into account, or that time-dependent ionization be considered. Thus plasma spectral models of general use need to be computed over a wide range of physical conditions.

  10. The estimation of the possibilities of synchrotron radiation X-ray fluorescent analysis and atomic specrometry for the bone's elemental composition determination

    NASA Astrophysics Data System (ADS)

    Gonchar, A. M.; Kolmogorov, U. P.; Gladkikh, E. A.; Shuvaeva, O. V.; Beisel, N. F.; Kolosova, N. G.

    2005-05-01

    Possibilities of multielemental highly sensitive techniques of analysis have been studied: synchrotron radiation X-ray fluorescence analysis (SR XFA), and atomic emission spectrometry with inductively bound plasma (ISP) and atomic absorption spectrometry (AAS) with flame (air-acetylene) atomization for assay of element composition of bone tissue with minimal preparation procedure. Results of comparative studies of elemental composition of bone tissue samples from experimental animals with inherited accelerated aging (rats of OXYS strain) using the SR XFA, ISP and AAS techniques are presented. It is shown that there exists in principle a possibility of assay of 22 biologically important essential macro- and trace elements within the range of 1.0-100,000 μg/g with a mean square analysis error of no more them 10-15% when using SR XFA.

  11. In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

    SciTech Connect

    Devloo-Casier, Kilian Detavernier, Christophe; Dendooven, Jolien

    2014-01-15

    Atomic layer deposition (ALD) is a thin film deposition technique that has been studied with a variety of in situ techniques. By exploiting the high photon flux and energy tunability of synchrotron based x-rays, a variety of new in situ techniques become available. X-ray reflectivity, grazing incidence small angle x-ray scattering, x-ray diffraction, x-ray fluorescence, x-ray absorption spectroscopy, and x-ray photoelectron spectroscopy are reviewed as possible in situ techniques during ALD. All these techniques are especially sensitive to changes on the (sub-)nanometer scale, allowing a unique insight into different aspects of the ALD growth mechanisms.

  12. Effective X-ray beam size measurements of an X-ray tube and polycapillary X-ray lens system using a scanning X-ray fluorescence method

    NASA Astrophysics Data System (ADS)

    Gherase, Mihai R.; Vargas, Andres Felipe

    2017-03-01

    Size measurements of an X-ray beam produced by an integrated polycapillary X-ray lens (PXL) and X-ray tube system were performed by means of a scanning X-ray fluorescence (SXRF) method using three different metallic wires. The beam size was obtained by fitting the SXRF data with the analytical convolution between a Gaussian and a constant functions. For each chemical element in the wire an effective energy was calculated based on the incident X-ray spectrum and its photoelectric cross section. The proposed method can be used to measure the effective X-ray beam size in XRF microscopy studies.

  13. Surface-Enhanced X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Anderson, Mark

    2010-01-01

    Surface-enhanced x-ray fluorescence (SEn-XRF) spectroscopy is a form of surface- enhanced spectroscopy that was conceived as a means of obtaining greater sensitivity in x-ray fluorescence (XRF) spectroscopy. As such, SEn-XRF spectroscopy joins the ranks of such other, longer-wavelength surface-enhanced spectroscopies as those based on surface-enhanced Raman scattering (SERS), surface-enhanced resonance Raman scattering (SERRS), and surfaceenhanced infrared Raman absorption (SEIRA), which have been described in previous NASA Tech Briefs articles. XRF spectroscopy has been used in analytical chemistry for determining the elemental compositions of small samples. XRF spectroscopy is rapid and quantitative and has been applied to a variety of metal and mineralogical samples. The main drawback of XRF spectroscopy as practiced heretofore is that sensitivity has not been as high as required for some applications. In SEn-XRF as in the other surface-enhanced spectroscopies, one exploits several interacting near-field phenomena, occurring on nanotextured surfaces, that give rise to local concentrations of incident far-field illumination. In this case, the far-field illumination comes from an x-ray source. Depending on the chemical composition and the geometry of a given nanotextured surface, these phenomena could include the lightning-rod effect (concentration of electric fields at the sharpest points on needlelike surface features), surface plasmon resonances, and grazing incidence geometric effects. In the far field, the observable effect of these phenomena is an increase in the intensity of the spectrum of interest - in this case, the x-ray fluorescence spectrum of chemical elements of interest that may be present within a surface layer at distances no more than a few nanometers from the surface.

  14. Silver coins analyses by X-ray fluorescence methods.

    PubMed

    Torrisi, L; Italiano, A; Cutroneo, M; Gentile, C; Torrisi, A

    2013-01-01

    The investigation on the differences occurring in the manufacture of silver coins allows to get information on their elemental composition and represents a powerful support to the methodology to identify the producing technologies, workshops being also instrumental to distinguish between original and counterfeit ones. Aim of the present work is to study recent and old silver coins through non-destructive X-Ray Fluorescence (XRF) analysis. The XRF was applied to extend the analysis to the deepest layers of the coins; for surface layers an X-ray tube or an electron beam were employed to induce the atom fluorescence to obtain information on the surface elemental composition. Moreover, a detailed study has been performed to evaluate the influence of the surface curvature on the measurement, by deducing a proper corrective factor to keep into account in the data analysis. The elemental atomic composition was measured for each coin, mainly by means of the X-ray tube excitation for the bulk and the electron Scanning Electron Microscope (SEM) microbeam probe for the surface patina analysis. Ionization was induced by an X-ray tube using an Ag anode for the bulk and by an electron microprobe for the surface composition. X-ray detection was performed by using a semiconductor Si device cooled by a Peltier system. The Ag L-lines X-ray yield is affected by coin surface morphology and geometry. The comparison between coin spectra and standard samples, shows that the Ag quantitative analysis is influenced by error of the atomic concentration lower that 10%.

  15. Nondestructive characterization of municipal-solid-waste-contaminated surface soil by energy-dispersive X-ray fluorescence and low-Z (atomic number) particle electron probe X-ray microanalysis.

    PubMed

    Gupta, Dhrubajyoti; Ghosh, Rita; Mitra, Ajoy K; Roy, Subinit; Sarkar, Manoranjan; Chowdhury, Subhajit; Bhowmik, Asit; Mukhopadhyay, Ujjal; Maskey, Shila; Ro, Chul-Un

    2011-11-01

    The long-term environmental impact of municipal solid waste (MSW) landfilling is still under investigation due to the lack of detailed characterization studies. A MSW landfill site, popularly known as Dhapa, in the eastern fringe of the metropolis of Kolkata, India, is the subject of present study. A vast area of Dhapa, adjoining the current core MSW dump site and evolving from the raw MSW dumping in the past, is presently used for the cultivation of vegetables. The inorganic chemical characteristics of the MSW-contaminated Dhapa surface soil (covering a 2-km stretch of the area) along with a natural composite (geogenic) soil sample (from a small countryside farm), for comparison, were investigated using two complementary nondestructive analytical techniques, energy-dispersive X-ray fluorescence (EDXRF) for bulk analysis and low-Z (atomic number) particle electron probe X-ray microanalysis (low-Z particle EPMA) for single-particle analysis. The bulk concentrations of K, Rb, and Zr remain almost unchanged in all the soil samples. The Dhapa soil is found to be polluted with heavy metals such as Cu, Zn, and Pb (highly elevated) and Ti, Cr, Mn, Fe, Ni, and Sr (moderately elevated), compared to the natural countryside soil. These high bulk concentration levels of heavy metals were compared with the Ecological Soil Screening Levels for these elements (U.S. Environment Protection Agency) to assess the potential risk on the immediate biotic environment. Low-Z particle EPMA results showed that the aluminosilicate-containing particles were the most abundant, followed by SiO2, CaCO3-containing, and carbonaceous particles in the Dhapa samples, whereas in the countryside sample only aluminosilicate-containing and SiO2 particles were observed. The mineral particles encountered in the countryside sample are solely of geogenic origin, whereas those from the Dhapa samples seem to have evolved from a mixture of raw dumped MSW, urban dust, and other contributing factors such as wind

  16. [X-ray fluorescence analysis in archaeometry: application and expectation].

    PubMed

    Zhu, Jian; Mao, Zhen-wei; Zhang, Shi-ding

    2006-12-01

    This article describes the applications of X-ray fluorescence in archaeology research, including the appraisal, dating, provenance and mine material origin analysis of cultural relic, the study of manufacturing technics and production of cultural relic, etc. It also suggests some expectation and problems, in order to draw attention of X-ray fluorescence analysts and archaeologists, promote the in-depth development of X-ray fluorescence analysis application in archaeology research, and further make more contributions to Chinese archaeology research.

  17. Coded Aperture Imaging for Fluorescent X-rays-Biomedical Applications

    SciTech Connect

    Haboub, Abdel; MacDowell, Alastair; Marchesini, Stefano; Parkinson, Dilworth

    2013-06-01

    Employing a coded aperture pattern in front of a charge couple device pixilated detector (CCD) allows for imaging of fluorescent x-rays (6-25KeV) being emitted from samples irradiated with x-rays. Coded apertures encode the angular direction of x-rays and allow for a large Numerical Aperture x- ray imaging system. The algorithm to develop the self-supported coded aperture pattern of the Non Two Holes Touching (NTHT) pattern was developed. The algorithms to reconstruct the x-ray image from the encoded pattern recorded were developed by means of modeling and confirmed by experiments. Samples were irradiated by monochromatic synchrotron x-ray radiation, and fluorescent x-rays from several different test metal samples were imaged through the newly developed coded aperture imaging system. By choice of the exciting energy the different metals were speciated.

  18. Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

    NASA Astrophysics Data System (ADS)

    Papadopoulou, D. N.; Zachariadis, G. A.; Anthemidis, A. N.; Tsirliganis, N. C.; Stratis, J. A.

    2004-12-01

    Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level).

  19. Determination of Fe(II) and Fe(III) in small samples by microbore ion chromatography and photometric, atomic absorption spectrometry and total-reflection X-ray fluorescence detection

    NASA Astrophysics Data System (ADS)

    Sinner, T.; Hoffmann, P.; Ortner, H. M.

    1993-02-01

    Iron(II) and iron(III) are determined after separation on an ion Chromatographie column by various detection systems. "On-line" detection was achieved by the use of a photometer with a flow cell of 0.8 μl; for "off-line" detection, graphite furnace atomic absorption spectrometry or total-reflection X-ray fluorescence were used. The applicability of the methods is shown for standard solutions and atmospheric samples. As a typical result, 50 μg/l of iron can be determined in a 10 μl sample with a nucrobore ion chromatograph-photometer and atomic absorption system and 40 μg/l of iron in a microbore ion chromatograph-total-reflection X-ray fluorescence combination.

  20. Coded aperture imaging for fluorescent x-rays

    SciTech Connect

    Haboub, A.; MacDowell, A. A.; Marchesini, S.; Parkinson, D. Y.

    2014-06-15

    We employ a coded aperture pattern in front of a pixilated charge couple device detector to image fluorescent x-rays (6–25 KeV) from samples irradiated with synchrotron radiation. Coded apertures encode the angular direction of x-rays, and given a known source plane, allow for a large numerical aperture x-ray imaging system. The algorithm to develop and fabricate the free standing No-Two-Holes-Touching aperture pattern was developed. The algorithms to reconstruct the x-ray image from the recorded encoded pattern were developed by means of a ray tracing technique and confirmed by experiments on standard samples.

  1. [The X-Ray Fluorescence Spectrometer Based on Pyroelectric Effect].

    PubMed

    Dong, Yi-fan; Fan, Rui-rui; Guo, Dong-ya; Zhang, Chun-lei; Gao, Min; Wang, Jin-zhou; Liu, Ya-qing; Zhou, Da-wei; Wang, Huan-yu

    2016-02-01

    Pyroelectric X-ray generator is implemented, and an X-ray fluorescence spectrometer is accomplished by combining the pyroelectric X-ray generator with a high energy resolution silicon drift detector. Firstly, the parameters of the X-ray generator are decided by analyzing and calculating the influence of the thickness of the pyroelectriccrystal and the thickness of the target on emitted X-ray. Secondly, the emitted X-ray is measured. The energy of emitted X-ray is from 1 to 27 keV, containing the characteristic X-ray of Cu and Ta, and the max counting rate is more than 3 000 per second. The measurement also proves that the detector of the spectrometer has a high energy resolution which the FWMH is 210 eV at 8. 05 keV. Lastly, samples of Fe, Ti, Cr and high-Ti basalt are analyzed using the spectrometer, and the results are agreed with the elements of the samples. It shows that the spectrometer consisting of a pyroelectric X-ray generator and a silicon drift detector is effective for element analysis. Additionally, because each part of the spectrometer has a small volume, it can be easily modified to a portable one which is suitable for non-destructive, on-site and quick element analysis.

  2. Development of a coincidence system for the measurement of X-ray emission atomic parameters

    NASA Astrophysics Data System (ADS)

    Martínez, Filiberto; Miranda, Javier

    2013-07-01

    Preliminary results obtained in experiments carried out with an x-ray spectrometer built at the Instituto de Física for Atomic Physics and environmental sciences studies are presented. The experiments are based on a coincidence method for signals produced by LEGe and Si(Li) detectors. The x-ray fluorescence yields (ωLi) and Coster-Kronig transition probabilities (fij) for elements with 55 ≤ Z ≤ 60 are among the quantities of interest. The method is based on the simultaneous detection of K x-rays with the LEGe detector and the L x-rays with the Si(Li) detector. The primary radiation source is an x-ray tube with Rh anode. The system was tested with the coincidence of the L x-rays from Ce with its K line, demonstrating the feasibility of the experiments.

  3. Atomic tungsten for ultrafast hard X-ray generation.

    PubMed

    Shan, Fang; Couch, Vernon A; Guo, Ting

    2005-05-19

    High-resolution X-ray absorption measurements (with an accuracy of +/-0.3 eV) of ZnSO(4) (aq) were performed with ultrafast selected energy X-ray absorption spectroscopy (USEXAS) using a laser-driven tungsten target X-ray source. The results were used to determine the absolute spectral positions of characteristic emission lines. By comparing these positions to those predicted for the line emission from tungsten of different oxidation states using the Dirac-Fock formula, the tungsten species responsible for ultrafast hard X-ray generation were found to be tungsten atoms. This finding provides the first direct evidence to support the mechanism of X-ray generation via high-energy electrons interacting with tungsten atoms in the solid target.

  4. Compton spectra of atoms at high x-ray intensity

    NASA Astrophysics Data System (ADS)

    Son, Sang-Kil; Geffert, Otfried; Santra, Robin

    2017-03-01

    Compton scattering is the nonresonant inelastic scattering of an x-ray photon by an electron and has been used to probe the electron momentum distribution in gas-phase and condensed-matter samples. In the low x-ray intensity regime, Compton scattering from atoms dominantly comes from bound electrons in neutral atoms, neglecting contributions from bound electrons in ions and free (ionized) electrons. In contrast, in the high x-ray intensity regime, the sample experiences severe ionization via x-ray multiphoton multiple ionization dynamics. Thus, it becomes necessary to take into account all the contributions to the Compton scattering signal when atoms are exposed to high-intensity x-ray pulses provided by x-ray free-electron lasers (XFELs). In this paper, we investigate the Compton spectra of atoms at high x-ray intensity, using an extension of the integrated x-ray atomic physics toolkit, xatom. As the x-ray fluence increases, there is a significant contribution from ionized electrons to the Compton spectra, which gives rise to strong deviations from the Compton spectra of neutral atoms. The present study provides not only understanding of the fundamental XFEL–matter interaction but also crucial information for single-particle imaging experiments, where Compton scattering is no longer negligible. , which features invited work from the best early-career researchers working within the scope of J. Phys. B. This project is part of the Journal of Physics series’ 50th anniversary celebrations in 2017. Sang-Kil Son was selected by the Editorial Board of J. Phys. B as an Emerging Leader.

  5. Quo Vadis total reflection X-ray fluorescence?

    NASA Astrophysics Data System (ADS)

    Pahlke, Siegfried

    2003-12-01

    The multielement trace analytical method 'total reflection X-ray fluorescence' (TXRF) has become a successfully established method in the semiconductor industry, particularly, in the ultra trace element analysis of silicon wafer surfaces. TXRF applications can fulfill general industrial requirements on daily routine of monitoring wafer cleanliness up to 300 mm diameter under cleanroom conditions. Nowadays, TXRF and hyphenated TXRF methods such as 'vapor phase decomposition (VPD)-TXRF', i.e. TXRF with a preceding surface and acid digestion and preconcentration procedure, are automated routine techniques ('wafer surface preparation system', WSPS). A linear range from 10 8 to 10 14 [atoms/cm 2] for some elements is regularly controlled. Instrument uptime is higher than 90%. The method is not tedious and can automatically be operated for 24 h/7 days. Elements such as S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sn, Sb, Ba and Pb are included in the software for standard peak search. The detection limits of recovered elements are between 1×10 11 and 1×10 7 [atoms/cm 2] depending upon X-ray excitation energy and the element of interest. For the determination of low Z elements, i.e. Na, Al and Mg, TXRF has also been extended but its implementation for routine analysis needs further research. At present, VPD-TXRF determination of light elements is viable in a range of 10 9 [atoms/cm 2]. Novel detectors such as silicon drift detectors (SDD) with an active area of 5 mm 2, 10 mm 2 or 20 mm 2, respectively, and multi-array detectors forming up to 70 mm 2 are commercially available. The first SDD with 100 mm 2 (!) area and integrated backside FET is working under laboratory conditions. Applications of and comparison with ICP-MS, HR-ICP-MS and SR-TXRF, an extension of TXRF capabilities with an extremely powerful energy source, are also reported.

  6. Remote X-Ray Diffraction and X-Ray Fluorescence Analysis on Planetary Surfaces

    NASA Technical Reports Server (NTRS)

    Blake, David F.; DeVincenzi, D. (Technical Monitor)

    1999-01-01

    The legacy of planetary X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) began in 1960 when W. Parish proposed an XRD instrument for deployment on the moon. The instrument was built and flight qualified, but the Lunar XRD program was cancelled shortly before the first human landing in 1969. XRF chemical data have been collected in situ by surface landers on Mars (Viking 1 & 2, Pathfinder) and Venus (Venera 13 & 14). These highly successful experiments provide critical constraints on our current understanding of surface processes and planetary evolution. However, the mineralogy, which is more critical to planetary surface science than simple chemical analysis, will remain unknown or will at best be imprecisely constrained until X-ray diffraction (XRD) data are collected. Recent progress in X-ray detector technology allows the consideration of simultaneous XRD (mineralogic analysis) and high-precision XRF (elemental analysis) in systems miniaturized to the point where they can be mounted on fixed landers or small robotic rovers. There is a variety of potential targets for XRD/XRF equipped landers within the solar system, the most compelling of which are the poles of the moon, the southern highlands of Mars and Europa.

  7. X-ray fluorescence analysis of various alloys. Part 1

    SciTech Connect

    Charles, J.W. Jr.; Ferguson, M.R.; Eager, M.H.

    1980-02-15

    For a number of years, x-ray fluorescence spectrometry has been used in the Y-12 Plant Laboratory for the analysis of a wide variety of materials. During the past few years, the technique has been applied to the analysis of a large number of experimental alloys. The general procedure consists of the following steps: (1) ignition of the alloy to oxides, (2) addition of suitable internal standards, (3) dissolution of the oxides and internal standards by sodium tetraborate (borax) fusion, (4) casting a pellet from the fusion in a graphite mold (Figure 1), and (5) determination of the major constituents by x-ray fluorescence spectrometry.

  8. 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

    NASA Astrophysics Data System (ADS)

    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.

  9. MSL Chemistry and Mineralogy X-Ray Diffraction X-Ray Fluorescence (CheMin) Instrument

    NASA Technical Reports Server (NTRS)

    Zimmerman, Wayne; Blake, Dave; Harris, William; Morookian, John Michael; Randall, Dave; Reder, Leonard J.; Sarrazin, Phillipe

    2013-01-01

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy Xray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

  10. HIgh Rate X-ray Fluorescence Detector

    SciTech Connect

    Grudberg, Peter Matthew

    2013-04-30

    The purpose of this project was to develop a compact, modular multi-channel x-ray detector with integrated electronics. This detector, based upon emerging silicon drift detector (SDD) technology, will be capable of high data rate operation superior to the current state of the art offered by high purity germanium (HPGe) detectors, without the need for liquid nitrogen. In addition, by integrating the processing electronics inside the detector housing, the detector performance will be much less affected by the typically noisy electrical environment of a synchrotron hutch, and will also be much more compact than current systems, which can include a detector involving a large LN2 dewar and multiple racks of electronics. The combined detector/processor system is designed to match or exceed the performance and features of currently available detector systems, at a lower cost and with more ease of use due to the small size of the detector. In addition, the detector system is designed to be modular, so a small system might just have one detector module, while a larger system can have many you can start with one detector module, and add more as needs grow and budget allows. The modular nature also serves to simplify repair. In large part, we were successful in achieving our goals. We did develop a very high performance, large area multi-channel SDD detector, packaged with all associated electronics, which is easy to use and requires minimal external support (a simple power supply module and a closed-loop water cooling system). However, we did fall short of some of our stated goals. We had intended to base the detector on modular, large-area detectors from Ketek GmbH in Munich, Germany; however, these were not available in a suitable time frame for this project, so we worked instead with pnDetector GmbH (also located in Munich). They were able to provide a front-end detector module with six 100 m^2 SDD detectors (two monolithic arrays of three elements each) along with

  11. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    NASA Technical Reports Server (NTRS)

    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. The Mapping X-Ray Fluorescence Spectrometer (MAPX)

    NASA Technical Reports Server (NTRS)

    Blake, David; Sarrazin, Philippe; Bristow, Thomas; Downs, Robert; Gailhanou, Marc; Marchis, Franck; Ming, Douglas; Morris, Richard; Sole, Vincente Armando; Thompson, Kathleen; Walter, Philippe; Wilson, Michael; Yen, Albert; Webb, Samuel

    2016-01-01

    MapX will provide elemental imaging at =100 micron spatial resolution over 2.5 X 2.5 centimeter areas, yielding elemental chemistry at or below the scale length where many relict physical, chemical, and biological features can be imaged and interpreted in ancient rocks. MapX is a full-frame spectroscopic imager positioned on soil or regolith with touch sensors. During an analysis, an X-ray source (tube or radioisotope) bombards the sample surface with X-rays or alpha-particles / gamma rays, resulting in sample X-ray Fluorescence (XRF). Fluoresced X-rays pass through an X-ray lens (X-ray µ-Pore Optic, "MPO") that projects a spatially resolved image of the X-rays onto a CCD. The CCD is operated in single photon counting mode so that the positions and energies of individual photons are retained. In a single analysis, several thousand frames are stored and processed. A MapX experiment provides elemental maps having a spatial resolution of =100 micron and quantitative XRF spectra from Regions of Interest (ROI) 2 centimers = x = 100 micron. ROI are compared with known rock and mineral compositions to extrapolate the data to rock types and putative mineralogies. The MapX geometry is being refined with ray-tracing simulations and with synchrotron experiments at SLAC. Source requirements are being determined through Monte Carlo modeling and experiment using XMIMSIM [1], GEANT4 [2] and PyMca [3] and a dedicated XRF test fixture. A flow-down of requirements for both tube and radioisotope sources is being developed from these experiments. In addition to Mars lander and rover missions, MapX could be used for landed science on other airless bodies (Phobos/Deimos, Comet nucleus, asteroids, the Earth's moon, and the icy satellites of the outer planets, including Europa.

  13. Computer simulation of a backscattered X-ray fluorescence system.

    PubMed

    Al-Ghorabie, Fayez H H

    2015-01-01

    An EGSnrc user code is developed to simulate a backscattered geometry in vivo x-ray fluorescence system for the measurement of platinum concentration in head and neck tumours. The user code is fundamentally based on a previous study which used the EGS4 Monte Carlo code. The new user code, which we have developed in this study, has new improvements which made it able to simulate the process of photon transportation through the different components of the modelled x-ray fluorescence system. The simulation process included modelling of the photon source, collimators, phantoms and detector. Simulation results were compared and evaluated against x-ray fluorescence data obtained experimentally from an existing system developed by the Swansea In vivo Analysis and Cancer Research Group. In addition, simulation results of this study were also compared with our previous study in which the EGS4 user code was used. Comparison between results has shown that the new EGSnrc user code was able to reproduce the spectral shape obtained using the experimental x-ray fluorescence system. The area under the Compton peak differs by 2.5% between the experimental measurement and the EGSnrc simulation. Similarly, the area under the two Pt Kα peaks differs by 2.3% and 2.2%.

  14. Measuring and interpreting X-ray fluorescence from planetary surfaces.

    PubMed

    Owens, Alan; Beckhoff, Burkhard; Fraser, George; Kolbe, Michael; Krumrey, Michael; Mantero, Alfonso; Mantler, Michael; Peacock, Anthony; Pia, Maria-Grazia; Pullan, Derek; Schneider, Uwe G; Ulm, Gerhard

    2008-11-15

    As part of a comprehensive study of X-ray emission from planetary surfaces and in particular the planet Mercury, we have measured fluorescent radiation from a number of planetary analog rock samples using monochromatized synchrotron radiation provided by the BESSY II electron storage ring. The experiments were carried out using a purpose built X-ray fluorescence (XRF) spectrometer chamber developed by the Physikalisch-Technische Bundesanstalt, Germany's national metrology institute. The XRF instrumentation is absolutely calibrated and allows for reference-free quantitation of rock sample composition, taking into account secondary photon- and electron-induced enhancement effects. The fluorescence data, in turn, have been used to validate a planetary fluorescence simulation tool based on the GEANT4 transport code. This simulation can be used as a mission analysis tool to predict the time-dependent orbital XRF spectral distributions from planetary surfaces throughout the mapping phase.

  15. X-ray fluorescence microscopy of olfactory receptor neurons

    NASA Astrophysics Data System (ADS)

    Dučić, T.; Breunig, E.; Schild, D.; Herbst, J.; Nováková, E.; Susini, J.; Tucoulu, R.; Salditt, T.

    2009-09-01

    We report a x-ray fluorescence microscopy study of cells and tissues from the olfactory system of Xenopus laevis. In this experiment we focus on sample preparation and experimental issues, and present first results of fluorescence maps of the elemental distribution of Cl, K, Ca, P, S and Na both in individual isolated neural cells and in cross-sections of the same tissue.

  16. Atomic Data Needs for X-Ray Astronomy

    NASA Technical Reports Server (NTRS)

    Kallman, Timothy; White, Nicholas E. (Technical Monitor)

    1999-01-01

    This publication contains written versions of most of the invited talks presented at the workshop on Atomic Data Needs for X-ray Astronomy which was held at NASA's Goddard Space Flight Center on December 16-1 7 1999. The idea of hosting such a workshop emerged from an imminent need to update and complete current atomic datasets in anticipation of a new era of high quality X-ray spectra starting with the launching of Chandra and XMM-Newton observatories. At first, our vision of the workshop was of a short and limited attendance event, given the specialization of the topic. But it, was soon realized, from the response to the first workshop announcement, that the topic was of much interest, to researchers working in X-ray spectra (physicists and astronomers). As a result, the workshop grew to approximately 120 participants from several countries. The kind of atomic data that interests us are those parameters needed for analysis and modeling of spectra shortward of about about 100 A and relevant to ionic species of astronomical interest. The physical mechanisms of interest in the formation of spectra include photoionization. collisional ionization, recombination (radiative and dielectronic). collisional excitation (by electrons and protons). and radiative deexcitation. Unique to X-ray spectroscopy are the ionization and excitation processes from inner-closed shells. in addition to the challenges in interpret,ing the medium resolution (epsilon/delta epsilon is about 0.05 - 0.1) data obtained by current X-ray astronomy experiments. Line wavelengths are of interest too, particularly owing to the high resolution spectra from the new experiments. The workshop was divided into five major areas: Observational Spectroscopy, Theoretical Calculations of Atomic Data, Laboratory Measurements of Atomic Parameters. Spectra Modeling, and Atomic Databases. One comforting finding from the work shop is that the enthusiasm felt by X-ray astronomers about the new observational missions

  17. X-ray absorption and soft x-ray fluorescence analysis of KDP optics

    SciTech Connect

    Nelson, A J; van Buuren, T; Miller, E; Land, T A; Bostedt, C; Franco, N; Whitman, P K; Baisden, P A; Terminello, L J; Callcott, T A

    2000-08-09

    Potassium Dihydrogen Phosphate (KDP) is a non-linear optical material used for laser frequency conversion and optical switches. Unfortunately, when KDP crystals are coated with a porous silica anti-reflection coating [1] and then exposed to ambient humidity, they develop dissolution pits [2,3]. Previous investigations [2] have shown that thermal annealing renders KDP optics less susceptible to pitting suggesting that a modification of surface chemistry has occurred. X-ray absorption and fluorescence were used to characterize changes in the composition and structure of KDP optics as a function of process parameters. KDP native crystals were also analyzed to provide a standard basis for interpretation. Surface sensitive total electron yield and bulk sensitive fluorescence yield from the K 2p, P 2p (L{sub 2,3}-edge) and O 1s (K-edge) absorption edges were measured at each process step. Soft X-ray fluorescence was also used to observe changes associated with spectral differences noted in the absorption measurements. Results indicate that annealing at 160 C dehydrates the surface of KDP resulting in a metaphosphate surface composition with K:P:O = 1:1:3.

  18. Atomic Data Needs for X-ray Astronomy

    NASA Technical Reports Server (NTRS)

    Bautista, Manuel A. (Editor); Kallman, Timothy R. (Editor); Pradhan, Anil K. (Editor)

    2000-01-01

    This publication contains written versions of most of the invited talks presented at the workshop on "Atomic Data Needs for X-ray Astronomy," which was held at NASA's Goddard Space Flight Center on December 16-17, 1999. The workshop was divided into five major areas: Observational Spectroscopy, Theoretical Calculations of Atomic Data, Laboratory Measurements of Atomic Parameters, Spectra Modeling, and Atomic Databases. These proceedings are expected to be of interest to producers and users of atomic data. Moreover, the contributions presented here have been written in a way that can be used by a general audience of scientists and graduate students in X-ray astronomy, modelling, and in computational and experimental atomic physics.

  19. X-ray fluorescence measurements of dissolved gas and cavitation

    NASA Astrophysics Data System (ADS)

    Duke, Daniel J.; Kastengren, Alan L.; Swantek, Andrew B.; Matusik, Katarzyna E.; Powell, Christopher F.

    2016-10-01

    The dynamics of dissolved gas and cavitation are strongly coupled, yet these phenomena are difficult to measure in-situ. Both create voids in the fluid that can be difficult to distinguish. We present an application of X-ray fluorescence in which liquid density and total noncondensible gas concentration (both dissolved and nucleated) are simultaneously measured. The liquid phase is doped with 400 ppm of a bromine tracer, and dissolved air is removed and substituted with krypton. Fluorescent emission at X-ray wavelengths is simultaneously excited from the Br and Kr with a focused monochromatic X-ray beam from a synchrotron source. We measure the flow in a cavitating nozzle 0.5 mm in diameter. From Br fluorescence, total displacement of the liquid is measured. From Kr fluorescence, the mass fraction of both dissolved and nucleated gas is measured. Volumetric displacement of liquid due to both cavitation and gas precipitation can be separated through estimation of the local equilibrium dissolved mass fraction. The uncertainty in the line of sight projected densities of the liquid and gas phases is 4-6 %. The high fluorescence yields and energies of Br and Kr allow small mass fractions of gas to be measured, down to 10-5, with an uncertainty of 8 %. These quantitative measurements complement existing optical diagnostic techniques and provide new insight into the diffusion of gas into cavitation bubbles, which can increase their internal density, pressure and lifetimes by orders of magnitude.

  20. X-ray fluorescence measurements of dissolved gas and cavitation

    SciTech Connect

    Duke, Daniel J.; Kastengren, Alan L.; Swantek, Andrew B.; Matusik, Katarzyna E.; Powell, Christopher F.

    2016-09-28

    The dynamics of dissolved gas and cavitation are strongly coupled, yet these phenomena are difficult to measure in-situ. Both create voids in the fluid that can be difficult to distinguish. In this paper, we present an application of X-ray fluorescence in which liquid density and total noncondensible gas concentration (both dissolved and nucleated) are simultaneously measured. The liquid phase is doped with 400 ppm of a bromine tracer, and dissolved air is removed and substituted with krypton. Fluorescent emission at X-ray wavelengths is simultaneously excited from the Br and Kr with a focused monochromatic X-ray beam from a synchrotron source. We measure the flow in a cavitating nozzle 0.5 mm in diameter. From Br fluorescence, total displacement of the liquid is measured. From Kr fluorescence, the mass fraction of both dissolved and nucleated gas is measured. Volumetric displacement of liquid due to both cavitation and gas precipitation can be separated through estimation of the local equilibrium dissolved mass fraction. The uncertainty in the line of sight projected densities of the liquid and gas phases is 4–6 %. The high fluorescence yields and energies of Br and Kr allow small mass fractions of gas to be measured, down to 10-5, with an uncertainty of 8 %. Finally, these quantitative measurements complement existing optical diagnostic techniques and provide new insight into the diffusion of gas into cavitation bubbles, which can increase their internal density, pressure and lifetimes by orders of magnitude.

  1. Water analysis via portable X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Pearson, Delaina; Chakraborty, Somsubhra; Duda, Bogdan; Li, Bin; Weindorf, David C.; Deb, Shovik; Brevik, Eric; Ray, D. P.

    2017-01-01

    Rapid, in-situ elemental water analysis would be an invaluable tool in studying polluted and/or salt-impacted waters. Analysis of water salinity has commonly used electrical conductance (EC); however, the identity of the elements responsible for the salinity are not revealed using EC. Several studies have established the viability of using portable X-ray fluorescence (PXRF) spectrometry for elemental data analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study used PXRF elemental data in water samples to predict water EC. A total of 256 water samples, from 10 different countries were collected and analyzed via PXRF, inductively coupled plasma atomic emission spectroscopy (ICP-AES), and a digital salinity bridge. The PXRF detected some elements more effectively than others, but overall results indicated that PXRF can successfully predict water EC via quantifying Cl in water samples (validation R2 and RMSE of 0.77 and 0.95 log μS cm-1, respectively). The findings of this study elucidated the potential of PXRF for future analysis of pollutant and/or metal contaminated waters.

  2. High-spatial-resolution nanoparticle x-ray fluorescence tomography

    NASA Astrophysics Data System (ADS)

    Larsson, Jakob C.; Vâgberg, William; Vogt, Carmen; Lundström, Ulf; Larsson, Daniel H.; Hertz, Hans M.

    2016-03-01

    X-ray fluorescence tomography (XFCT) has potential for high-resolution 3D molecular x-ray bio-imaging. In this technique the fluorescence signal from targeted nanoparticles (NPs) is measured, providing information about the spatial distribution and concentration of the NPs inside the object. However, present laboratory XFCT systems typically have limited spatial resolution (>1 mm) and suffer from long scan times and high radiation dose even at high NP concentrations, mainly due to low efficiency and poor signal-to-noise ratio. We have developed a laboratory XFCT system with high spatial resolution (sub-100 μm), low NP concentration and vastly decreased scan times and dose, opening up the possibilities for in-vivo small-animal imaging research. The system consists of a high-brightness liquid-metal-jet microfocus x-ray source, x-ray focusing optics and an energy-resolving photon-counting detector. By using the source's characteristic 24 keV line-emission together with carefully matched molybdenum nanoparticles the Compton background is greatly reduced, increasing the SNR. Each measurement provides information about the spatial distribution and concentration of the Mo nanoparticles. A filtered back-projection method is used to produce the final XFCT image.

  3. Methodology using a portable X-ray fluorescence device for on-site and rapid evaluation of heavy-atom contamination in wounds: a model study for application to plutonium contamination.

    PubMed

    Yoshii, Hiroshi; Yanagihara, Kouta; Imaseki, Hitoshi; Hamano, Tsuyoshi; Yamanishi, Hirokuni; Inagaki, Masayo; Sakai, Yasuhiro; Sugiura, Nobuyuki; Kurihara, Osamu; Sakai, Kazuo

    2014-01-01

    Workers decommissioning the Fukushima-Daiichi nuclear power plant damaged from the Great East Japan Earthquake and resulting tsunami are at risk of injury with possible contamination from radioactive heavy atoms including actinides, such as plutonium. We propose a new methodology for on-site and rapid evaluation of heavy-atom contamination in wounds using a portable X-ray fluorescence (XRF) device. In the present study, stable lead was used as the model contaminant substitute for radioactive heavy atoms. First, the wound model was developed by placing a liquid blood phantom on an epoxy resin wound phantom contaminated with lead. Next, the correlation between the concentration of contaminant and the XRF peak intensity was formulated considering the thickness of blood exiting the wound. Methods to determine the minimum detection limit (MDL) of contaminants at any maximal equivalent dose to the wound by XRF measurement were also established. For example, in this system, at a maximal equivalent dose of 16.5 mSv to the wound and blood thickness of 0.5 mm, the MDL value for lead was 1.2 ppm (3.1 nmol). The radioactivity of 239Pu corresponding to 3.1 nmol is 1.7 kBq, which is lower than the radioactivity of 239Pu contaminating puncture wounds in previous severe accidents. In conclusion, the established methodology could be beneficial for future development of a method to evaluate plutonium contamination in wounds. Highlights: Methodology for evaluation of heavy-atom contamination in a wound was established. A portable X-ray fluorescence device enables on-site, rapid and direct evaluation. This method is expected to be used for evaluation of plutonium contamination in wounds.

  4. Methodology Using a Portable X-Ray Fluorescence Device for On-Site and Rapid Evaluation of Heavy-Atom Contamination in Wounds: A Model Study for Application to Plutonium Contamination

    PubMed Central

    Yoshii, Hiroshi; Yanagihara, Kouta; Imaseki, Hitoshi; Hamano, Tsuyoshi; Yamanishi, Hirokuni; Inagaki, Masayo; Sakai, Yasuhiro; Sugiura, Nobuyuki; Kurihara, Osamu; Sakai, Kazuo

    2014-01-01

    Workers decommissioning the Fukushima-Daiichi nuclear power plant damaged from the Great East Japan Earthquake and resulting tsunami are at risk of injury with possible contamination from radioactive heavy atoms including actinides, such as plutonium. We propose a new methodology for on-site and rapid evaluation of heavy-atom contamination in wounds using a portable X-ray fluorescence (XRF) device. In the present study, stable lead was used as the model contaminant substitute for radioactive heavy atoms. First, the wound model was developed by placing a liquid blood phantom on an epoxy resin wound phantom contaminated with lead. Next, the correlation between the concentration of contaminant and the XRF peak intensity was formulated considering the thickness of blood exiting the wound. Methods to determine the minimum detection limit (MDL) of contaminants at any maximal equivalent dose to the wound by XRF measurement were also established. For example, in this system, at a maximal equivalent dose of 16.5 mSv to the wound and blood thickness of 0.5 mm, the MDL value for lead was 1.2 ppm (3.1 nmol). The radioactivity of 239Pu corresponding to 3.1 nmol is 1.7 kBq, which is lower than the radioactivity of 239Pu contaminating puncture wounds in previous severe accidents. In conclusion, the established methodology could be beneficial for future development of a method to evaluate plutonium contamination in wounds. Highlights: Methodology for evaluation of heavy-atom contamination in a wound was established. A portable X-ray fluorescence device enables on-site, rapid and direct evaluation. This method is expected to be used for evaluation of plutonium contamination in wounds. PMID:25010749

  5. Development and applications of grazing exit micro X-ray fluorescence instrument using a polycapillary X-ray lens*1

    NASA Astrophysics Data System (ADS)

    Emoto, T.; Sato, Y.; Konishi, Y.; Ding, X.; Tsuji, K.

    2004-08-01

    A polycapillary X-ray lens is an effective optics to obtain a μm-size X-ray beam for micro-X-ray fluorescence spectrometry (μ-XRF). We developed a μ-XRF instrument using a polycapillary X-ray lens, which also enabled us to perform Grazing Exit μ-XRF (GE-μ-XRF). The evaluated diameter of the primary X-ray beam was 48 μm at the focal distance of the X-ray lens. Use of this instrument enabled two-dimensional mapping of the elemental distributions during growth of the plant "Quinoa". The results of the mapping revealed elemental transition during growth. In addition, a small region of thin film was analyzed by GE-μ-XRF. We expect that GE-μ-XRF will become an effective method of estimating the film thickness of a small region.

  6. Proton-induced x-ray fluorescence CT imaging

    SciTech Connect

    Bazalova-Carter, Magdalena Xing, Lei; Ahmad, Moiz; Matsuura, Taeko; Takao, Seishin; Shirato, Hiroki; Umegaki, Kikuo; Matsuo, Yuto; Fahrig, Rebecca

    2015-02-15

    Purpose: To demonstrate the feasibility of proton-induced x-ray fluorescence CT (pXFCT) imaging of gold in a small animal sized object by means of experiments and Monte Carlo (MC) simulations. Methods: First, proton-induced gold x-ray fluorescence (pXRF) was measured as a function of gold concentration. Vials of 2.2 cm in diameter filled with 0%–5% Au solutions were irradiated with a 220 MeV proton beam and x-ray fluorescence induced by the interaction of protons, and Au was detected with a 3 × 3 mm{sup 2} CdTe detector placed at 90° with respect to the incident proton beam at a distance of 45 cm from the vials. Second, a 7-cm diameter water phantom containing three 2.2-diameter vials with 3%–5% Au solutions was imaged with a 7-mm FWHM 220 MeV proton beam in a first generation CT scanning geometry. X-rays scattered perpendicular to the incident proton beam were acquired with the CdTe detector placed at 45 cm from the phantom positioned on a translation/rotation stage. Twenty one translational steps spaced by 3 mm at each of 36 projection angles spaced by 10° were acquired, and pXFCT images of the phantom were reconstructed with filtered back projection. A simplified geometry of the experimental data acquisition setup was modeled with the MC TOPAS code, and simulation results were compared to the experimental data. Results: A linear relationship between gold pXRF and gold concentration was observed in both experimental and MC simulation data (R{sup 2} > 0.99). All Au vials were apparent in the experimental and simulated pXFCT images. Specifically, the 3% Au vial was detectable in the experimental [contrast-to-noise ratio (CNR) = 5.8] and simulated (CNR = 11.5) pXFCT image. Due to fluorescence x-ray attenuation in the higher concentration vials, the 4% and 5% Au contrast were underestimated by 10% and 15%, respectively, in both the experimental and simulated pXFCT images. Conclusions: Proton-induced x-ray fluorescence CT imaging of 3%–5% gold solutions in a

  7. Proton-induced x-ray fluorescence CT imaging

    PubMed Central

    Bazalova-Carter, Magdalena; Ahmad, Moiz; Matsuura, Taeko; Takao, Seishin; Matsuo, Yuto; Fahrig, Rebecca; Shirato, Hiroki; Umegaki, Kikuo; Xing, Lei

    2015-01-01

    Purpose: To demonstrate the feasibility of proton-induced x-ray fluorescence CT (pXFCT) imaging of gold in a small animal sized object by means of experiments and Monte Carlo (MC) simulations. Methods: First, proton-induced gold x-ray fluorescence (pXRF) was measured as a function of gold concentration. Vials of 2.2 cm in diameter filled with 0%–5% Au solutions were irradiated with a 220 MeV proton beam and x-ray fluorescence induced by the interaction of protons, and Au was detected with a 3 × 3 mm2 CdTe detector placed at 90° with respect to the incident proton beam at a distance of 45 cm from the vials. Second, a 7-cm diameter water phantom containing three 2.2-diameter vials with 3%–5% Au solutions was imaged with a 7-mm FWHM 220 MeV proton beam in a first generation CT scanning geometry. X-rays scattered perpendicular to the incident proton beam were acquired with the CdTe detector placed at 45 cm from the phantom positioned on a translation/rotation stage. Twenty one translational steps spaced by 3 mm at each of 36 projection angles spaced by 10° were acquired, and pXFCT images of the phantom were reconstructed with filtered back projection. A simplified geometry of the experimental data acquisition setup was modeled with the MC TOPAS code, and simulation results were compared to the experimental data. Results: A linear relationship between gold pXRF and gold concentration was observed in both experimental and MC simulation data (R2 > 0.99). All Au vials were apparent in the experimental and simulated pXFCT images. Specifically, the 3% Au vial was detectable in the experimental [contrast-to-noise ratio (CNR) = 5.8] and simulated (CNR = 11.5) pXFCT image. Due to fluorescence x-ray attenuation in the higher concentration vials, the 4% and 5% Au contrast were underestimated by 10% and 15%, respectively, in both the experimental and simulated pXFCT images. Conclusions: Proton-induced x-ray fluorescence CT imaging of 3%–5% gold solutions in a small animal

  8. Elemental analysis using a handheld X-Ray fluorescence spectrometer

    USGS Publications Warehouse

    Groover, Krishangi D.; Izbicki, John

    2016-06-24

    The U.S. Geological Survey is collecting geologic samples from local stream channels, aquifer materials, and rock outcrops for studies of trace elements in the Mojave Desert, southern California. These samples are collected because geologic materials can release a variety of elements to the environment when exposed to water. The samples are to be analyzed with a handheld X-ray fluorescence (XRF) spectrometer to determine the concentrations of up to 27 elements, including chromium.

  9. Identifications studies of Lauha Bhasma by X-ray diffraction and X-ray fluorescence.

    PubMed

    Bhargava, S C; Reddy, K R C; Sastry, G V S

    2012-01-01

    Procedures for preparation of Lauha Bhasma are described in ancient texts of Ayurveda. These procedures also begin with different source material for iron such as Teekshna Lauha and Kanta Lauha etc. In the present study, we have selected different source materials viz. magnetite iron ore for Kanta Lauha and pure (Armco grade) iron turnings for Teekshna Lauha. The standard procedures of preparation of Lauha Bhasma are carried out in identical conditions for these two raw materials. The final product from the Puta are characterized by using X-ray diffraction and X-ray fluorescence spectroscopy to understanding the crystallographic form or forms of iron oxides and their composition at the end of each Puta. The iron content at the end of repeated Putas (18 for Kanta Lauha and 20 for Teekshna Lauha) have shown a decrease in case of Teekshna Lauha since the starting material is pure iron while it showed only marginal decreases in the case of Kanta Lauha because the Fe(3)O(4) of magnetite is undergoing oxidation to Fe(2)O(3). The trace elements remain within the Bhasma in the form of various oxides of Si, Al, Ca, etc.

  10. Determination of regional myocardial perfusion by x-ray fluorescence

    SciTech Connect

    Palmer, B.M.; McInerney, J.J. )

    1990-05-01

    Validation studies were performed to demonstrate the effectiveness of an x-ray induced fluorescence system in quantitating regional myocardial perfusion in vivo. In a series of 13 open-chested canines, x-ray induced fluorescence was used to simultaneously monitor iodine concentration transients which arose in the left ventricular lumen and in the myocardium after the intravenous injection of an iodinated flow tracer. Deconvolution of the recorded transients produced a transfer function from which the mean transit time for the tracer to travel between the left ventricular lumen and the myocardium was calculated. Measurements of regional myocardial perfusion (Q) made by radioactive microspheres were compared with the reciprocals of the mean transit times (MTT-1) and gave a linear correlation (n = 38): MTT-1 = 0.033 + 0.069 Q, r = 0.71. Comparison of the percent change in perfusion (dQ) relative to a control study for each dog with the percent change in the respective reciprocals of the mean transit times (dMTT-1) produced a linear correlation coefficient of r = 0.88 for the regression line dMTT-1 = 0.46 dQ - 10.7. The x-ray induced fluorescence system may provide a minimally invasive means for monitoring iodine concentration transients and determining relative, if not absolute, measures of regional myocardial perfusion.

  11. Calculating the X-Ray Fluorescence from the Planet Mercury Due to High-Energy Electrons

    NASA Technical Reports Server (NTRS)

    Burbine, T. H.; Trombka, J. I.; Bergstrom, P. M., Jr.; Christon, S. P.

    2005-01-01

    The least-studied terrestrial planet is Mercury due to its proximity to the Sun, which makes telescopic observations and spacecraft encounters difficult. Our lack of knowledge about Mercury should change in the near future due to the recent launching of MESSENGER, a Mercury orbiter. Another mission (BepiColombo) is currently being planned. The x-ray spectrometer on MESSENGER (and planned for BepiColombo) can characterize the elemental composition of a planetary surface by measuring emitted fluorescent x-rays. If electrons are ejected from an atom s inner shell by interaction with energetic particles such as photons, electrons, or ions, electrons from an outer shell can transfer to the inner shell. Characteristic x-rays are then emitted with energies that are the difference between the binding energy of the ion in its excited state and that of the ion in its ground state. Because each element has a unique set of energy levels, each element emits x-rays at a unique set of energies. Electrons and ions usually do not have the needed flux at high energies to cause significant x-ray fluorescence on most planetary bodies. This is not the case for Mercury where high-energy particles were detected during the Mariner 10 flybys. Mercury has an intrinsic magnetic field that deflects the solar wind, resulting in a bow shock in the solar wind and a magnetospheric cavity. Electrons and ions accelerated in the magnetosphere tend to follow its magnetic field lines and can impact the surface on Mercury s dark side Modeling has been done to determine if x-ray fluorescence resulting from the impact of high-energy electrons accelerated in Mercury's magnetosphere can be detected by MESSENGER. Our goal is to understand how much bulk chemical information can be obtained from x-ray fluorescence measurements on the dark side of Mercury.

  12. Micro-X-ray Fluorescence (MXRF) Direct Solids

    SciTech Connect

    Worley, Christopher Gordon

    2015-03-04

    MXRF complements other imaging techniques such as SEM-EDS, and MXRF is a method of choice for: Large area analyses (up to 100 cm2 areas); True NDA – No damage from X-ray beam; Medium and high atomic number elemental analyses; Non-conducting materials (eg. plastics, HEPA filters, etc.); Samples incompatible with vacuum (eg. liquids, moist samples). Presented are several MXRF BSAP-related applications.

  13. Optical Fluorescence Detected from X-ray Irradiated Liquid Water.

    PubMed

    Hans, Andreas; Ozga, Christian; Seidel, Robert; Schmidt, Philipp; Ueltzhöffer, Timo; Holzapfel, Xaver; Wenzel, Philip; Reiß, Philipp; Pohl, Marvin N; Unger, Isaak; Aziz, Emad F; Ehresmann, Arno; Slavíček, Petr; Winter, Bernd; Knie, André

    2017-03-16

    Despite its importance, the structure and dynamics of liquid water are still poorly understood in many apsects. Here, we report on the observation of optical fluorescence upon soft X-ray irradiation of liquid water. Detection of spectrally resolved fluorescence was achieved by a combination of the liquid microjet technique and fluorescence spectroscopy. We observe a genuine liquid-phase fluorescence manifested by a broad emission band in the 170-340 nm (4-7 eV) photon wavelength range. In addition, another narrower emission near 300 nm can be assigned to the fluorescence of OH (A state) in the gas phase, the emitting species being formed by Auger electrons escaping from liquid water. We argue that the newly observed broad-band emission of liquid water is relevant in search of extraterrestrial life, and we also envision the observed electron-ejection mechanism to find application for exploring solutes at liquid-vapor interfaces.

  14. Proton induced quasi-monochromatic x-ray beams for soft x-ray spectroscopy studies and selective x-ray fluorescence analysis

    SciTech Connect

    Sokaras, D.; Zarkadas, Ch.; Fliegauf, R.; Beckhoff, B.; Karydas, A. G.

    2012-12-15

    We present the analytical features and performance of an x-ray spectroscopy end station of moderate energy resolution operating with proton-induced quasi-monochromatic x-ray beams. The apparatus was designed, installed and operated at the 5.5 MV Tandem VdG Accelerator Laboratory of the Institute of Nuclear Physics, N.C.S.R. 'Demokritos,' Athens. The setup includes a two-level ultrahigh vacuum chamber that hosts in the lower level up to six primary targets in a rotatable holder; there, the irradiation of pure element materials-used as primary targets-with few-MeV high current ({approx}{mu}A) proton beams produces intense quasi-monochromatic x-ray beams of selectable energy. In the chamber's upper level, a six-position rotatable sample holder hosts the targets considered for x-ray spectroscopy studies. The proton-induced x-ray beam, after proper collimation, is guided to the sample position whereas various filters can be also inserted along the beam's path to eliminate the backscattered protons or/and to absorb selectively components of the x-ray beam. The apparatus incorporates an ultrathin window Si(Li) spectrometer (FWHM 136 eV at 5.89 keV) coupled with low-noise electronics capable of efficiently detecting photons down to carbon K{alpha}. Exemplary soft x-ray spectroscopy studies and results of selective x-ray fluorescence analysis are presented.

  15. X-ray fluorescence measurements of dissolved gas and cavitation

    DOE PAGES

    Duke, Daniel J.; Kastengren, Alan L.; Swantek, Andrew B.; ...

    2016-09-28

    The dynamics of dissolved gas and cavitation are strongly coupled, yet these phenomena are difficult to measure in-situ. Both create voids in the fluid that can be difficult to distinguish. In this paper, we present an application of X-ray fluorescence in which liquid density and total noncondensible gas concentration (both dissolved and nucleated) are simultaneously measured. The liquid phase is doped with 400 ppm of a bromine tracer, and dissolved air is removed and substituted with krypton. Fluorescent emission at X-ray wavelengths is simultaneously excited from the Br and Kr with a focused monochromatic X-ray beam from a synchrotron source.more » We measure the flow in a cavitating nozzle 0.5 mm in diameter. From Br fluorescence, total displacement of the liquid is measured. From Kr fluorescence, the mass fraction of both dissolved and nucleated gas is measured. Volumetric displacement of liquid due to both cavitation and gas precipitation can be separated through estimation of the local equilibrium dissolved mass fraction. The uncertainty in the line of sight projected densities of the liquid and gas phases is 4–6 %. The high fluorescence yields and energies of Br and Kr allow small mass fractions of gas to be measured, down to 10-5, with an uncertainty of 8 %. Finally, these quantitative measurements complement existing optical diagnostic techniques and provide new insight into the diffusion of gas into cavitation bubbles, which can increase their internal density, pressure and lifetimes by orders of magnitude.« less

  16. NEW CORRECTION PROCEDURE FOR X-RAY SPECTROSCOPIC FLUORESCENCE DATA: SIMULATIONS AND EXPERIMENT.

    SciTech Connect

    ABLETT, J.M.; WOICIK, J.C.; KAO, C.C.

    2004-08-02

    X-ray fluorescence spectroscopy is a widely used method for determining the electronic configuration and local structure of dilute species with high sensitivity. In the dilute limit, and for thin films, the X-ray fluorescence signal is directly proportional to the atomic sub-shell absorption coefficient. However, for concentrated samples, the well-documented self-absorption effect often leads to the severe suppression of XANES (X-ray Absorption Near-Edge Structure) and EXAFS (Extended X-ray Absorption Fine-Structure) amplitudes. Thus to recover the real value of the sub-shell absorption coefficient, it is important to apply correction procedures to the measured fluorescence spectra. In this paper, we describe a new straightforward method to correct for self-absorption effects (the difference in the measured fluorescence signal compared to that of the true sub-shell photoabsorption coefficient) in XANES and EXAFS fluorescence measurements. Using a variety of sample and detector configurations, this method is used to extract the sub-shell absorption coefficient on elemental nickel and thick single-crystals of Gd{sub 3}Ga{sub 5}O{sub 12} and LaAlO{sub 3}.

  17. New Correction Procedure For X-ray Spectroscopic Fluorescence Data: Simulations and Experiment

    SciTech Connect

    Ablett,J.; Woicik, J.; Kao, C.

    2005-01-01

    X-ray fluorescence spectroscopy is a widely used method for determining the electronic configuration and local structure of dilute species with high sensitivity. In the dilute limit, and for thin films, the X-ray fluorescence signal is directly proportional to the atomic sub-shell absorption coefficient. However, for concentrated samples, the well-documented self-absorption effect often leads to the severe suppression of XANES (X-ray Absorption Near-Edge Structure) and EXAFS (Extended X-ray Absorption Fine-Structure) amplitudes. Thus to recover the real value of the sub-shell absorption coefficient, it is important to apply correction procedures to the measured fluorescence spectra. In this paper, we describe a new straightforward method to correct for self-absorption effects (the difference in the measured fluorescence signal compared to that of the true sub-shell photoabsorption coefficient) in XANES and EXAFS fluorescence measurements. Using a variety of sample and detector configurations, this method is used to extract the sub-shell absorption coefficient on elemental nickel and thick single-crystals of Gd{sub 3}Ga{sub 5}O{sub 12} and LaAlO{sub 3}.

  18. Micro-X-ray Fluorescence in Food Forensics

    NASA Astrophysics Data System (ADS)

    St. Jeor, V. L.; Muroski, A. R.; McGuire, C.; Lape, A.

    2011-09-01

    All forms of commercially available x-ray microscopy are finding growing application opportunities within the food industry; this includes micro-x-ray fluorescence (micro-XRF) and micro-CT. In this example, we demonstrate the use of micro-XRF in discovering the cause for a particularly troubling anomaly discovered by one of our customers during the production of a batch of their chicken hotdogs. Although their claim was that iron filings must be present to cause such anomalies, no "iron filings" were discovered in our initial observations. More traditional EDS methods were attempted to determine the elemental content within these anomalies, but they were not sensitive enough to detect the small amounts of iron that were, in fact, present. Nor could EDS determine the source for this minute amount of iron. Only micro-XRF displayed the required sensitivity to detect the iron and to make an initial diagnosis regarding its potential source. Visible spectroscopy confirms. Instrumentation is reviewed.

  19. Energetic electron processes fluorescence effects for structured nanoparticles X-ray analysis and nuclear medicine applications

    NASA Astrophysics Data System (ADS)

    Taborda, A.; Desbrée, A.; Carvalho, A.; Chaves, P. C.; Reis, M. A.

    2016-08-01

    Superparamagnetic iron oxide (SPIO) nanoparticles are widely used as contrast agents for nuclear magnetic resonance imaging (MRI), and can be modified for improved imaging or to become tissue-specific or even protein-specific. The knowledge of their detailed elemental composition characterisation and potential use in nuclear medicine applications, is, therefore, an important issue. X-ray fluorescence techniques such as particle induced X-ray emission (PIXE) or X-ray fluorescence spectrometry (XRF), can be used for elemental characterisation even in problematic situations where very little sample volume is available. Still, the fluorescence coefficient of Fe is such that, during the decay of the inner-shell ionised atomic structure, keV Auger electrons are produced in excess to X-rays. Since cross-sections for ionisation induced by keV electrons, for low atomic number atoms, are of the order of 103 barn, care should be taken to account for possible fluorescence effects caused by Auger electrons, which may lead to the wrong quantification of elements having atomic number lower than the atomic number of Fe. Furthermore, the same electron processes will occur in iron oxide nanoparticles containing 57Co, which may be used for nuclear medicine therapy purposes. In the present work, simple approximation algorithms are proposed for the quantitative description of radiative and non-radiative processes associated with Auger electrons cascades. The effects on analytical processes and nuclear medicine applications are quantified for the case of iron oxide nanoparticles, by calculating both electron fluorescence emissions and energy deposition on cell tissues where the nanoparticles may be embedded.

  20. High resolution x-ray fluorescence spectroscopy - a new technique for site- and spin-selectivity

    SciTech Connect

    Wang, Xin

    1996-12-01

    X-ray spectroscopy has long been used to elucidate electronic and structural information of molecules. One of the weaknesses of x-ray absorption is its sensitivity to all of the atoms of a particular element in a sample. Through out this thesis, a new technique for enhancing the site- and spin-selectivity of the x-ray absorption has been developed. By high resolution fluorescence detection, the chemical sensitivity of K emission spectra can be used to identify oxidation and spin states; it can also be used to facilitate site-selective X-ray Absorption Near Edge Structure (XANES) and site-selective Extended X-ray Absorption Fine Structure (EXAFS). The spin polarization in K fluorescence could be used to generate spin selective XANES or spin-polarized EXAFS, which provides a new measure of the spin density, or the nature of magnetic neighboring atoms. Finally, dramatic line-sharpening effects by the combination of absorption and emission processes allow observation of structure that is normally unobservable. All these unique characters can enormously simplify a complex x-ray spectrum. Applications of this novel technique have generated information from various transition-metal model compounds to metalloproteins. The absorption and emission spectra by high resolution fluorescence detection are interdependent. The ligand field multiplet model has been used for the analysis of K{alpha} and K{beta} emission spectra. First demonstration on different chemical states of Fe compounds has shown the applicability of site selectivity and spin polarization. Different interatomic distances of the same element in different chemical forms have been detected using site-selective EXAFS.

  1. Atomic holography with electrons and x-rays: Theoretical and experimental studies

    SciTech Connect

    Len, Patrick Michael

    1997-06-01

    Gabor first proposed holography in 1948 as a means to experimentally record the amplitude and phase of scattered wavefronts, relative to a direct unscattered wave, and to use such a "hologram" to directly image atomic structure. But imaging at atomic resolution has not yet been possible in the way he proposed. Much more recently, Szoeke in 1986 noted that photoexcited atoms can emit photoelectron of fluorescent x-ray wavefronts that are scattered by neighboring atoms, thus yielding the direct and scattered wavefronts as detected in the far field that can then be interpreted as holographic in nature. By now, several algorithms for directly reconstructing three-dimensional atomic images from electron holograms have been proposed (e.g. by Barton) and successfully tested against experiment and theory. Very recently, Tegze and Faigel, and Grog et al. have recorded experimental x-ray fluorescence holograms, and these are found to yield atomic images that are more free of the kinds of aberrations caused by the non-ideal emission or scattering of electrons. The basic principles of these holographic atomic imaging methods are reviewed, including illustrative applications of the reconstruction algorithms to both theoretical and experimental electron and x-ray holograms. The author also discusses the prospects and limitations of these newly emerging atomic structural probes.

  2. An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

    NASA Technical Reports Server (NTRS)

    Ross, H. Richard

    1993-01-01

    A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

  3. Analysis of Historical Coins by X-ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Raddell, Mark; Manukyan, Khatchatur; Aprahamian, Ani; Jordan, Louis

    2016-09-01

    Using different setups of the EDAX Orbis Micro X-ray Fluorescence (XRF) Analyzer, we have learned more about the limitations and optimizations of the XRF method and collected data about early British and Spanish colonial silver coins. XRF spectrometry was used to study Mexican, Bolivian, and Massachusetts silver coins from the University of Notre Dame's Rare Books and Special Collections Department. Runs were performed in both air and vacuum conditions, and the x-ray beam diameter was compared between 1 and 0.03 mm. Using these methods we were able to contribute to the understanding of the historical coinage as well as learn about the best ways to use the method. During analysis we found significant differences in the spectra for silver L shell excitation and silver K shell excitation when switching from 0.03 to 1mm x-ray beam widths. Our data trends also fit with the historical theory that the coinage from the Massachusetts' mint were created by melting down Spanish silver coins (like the ones made from Mexico and Bolivia) and adding a small percent more of copper. We have the intent to build on what we have learned by also studying some Roman Denarii in the future, and by trying to create a custom designed version of the XRF which can be moved more easily and provide quick scans for a larger number of artifacts.

  4. The Apollo 15 X-ray fluorescence experiment

    NASA Technical Reports Server (NTRS)

    Adler, I.; Trombka, J.; Gerard, J.; Schmadebeck, R.; Lowman, P.; Blodgett, H.; Yin, L.; Eller, E.; Lamothe, R.; Gorenstein, P.

    1972-01-01

    The CSM spectrometric data on the lunar surface with respect to its chemical composition are presented for Al, Mg, and Si as Al/Si and Mg/Si ratios for the various features overflow by the spacecraft. The lunar surface measurements involved observations of the intensity and characteristic energy distribution of the secondary or fluorescent X-rays produced by the interaction of solar X-rays with the lunar surface. The results showed that the highlands and maria are chemically different, with the highlands having considerably more Al and less Mg than the maria. The mare-highland contact is quite sharp and puts a limit on the amount of horizontal transport of material. The X-ray data suggest that the dominant rock type of the lunar highlands is a plagioclase-rich pyroxene bearing rock, probably anorthositic gabbro or feldspathic basalt. Thus the moon appears to have a widespread differentiated crust (the highlands) systematically richer in Al and lower in Mg than the maria. This crust is pre-mare and may represent the first major internal differentiation of the moon.

  5. X-ray fluorescence analysis of low concentrations metals in geological samples and technological products

    NASA Astrophysics Data System (ADS)

    Lagoida, I. A.; Trushin, A. V.

    2016-02-01

    For the past several years many nuclear physics methods of quantitative elemental analysis have been designed. Many of these methods have applied in different devices which have become useful and effective instrument in many industrial laboratories. Methods of a matter structure analysis are based on the intensity detection of the X-ray radiation from the nuclei of elements which are excited by external X-ray source. The production of characteristic X-rays involves transitions of the orbital electrons of atoms in the target material between allowed orbits, or energy states, associated with ionization of the inner atomic shells. One of these methods is X-ray fluorescence analysis, which is widespread in metallurgical and processing industries and is used to identify and measure the concentration of the elements in ores and minerals on a conveyor belt. Samples of copper ore with known concentrations of elements, were taken from the Ural deposit. To excite the characteristic X-rays radionuclide sources 109Cd, with half-life 461.4 days were used. After finding the calibration coefficients, control measurements of samples and averaging of overall samples were made. The measurement error did not exceed 3%.

  6. Simultaneous X-ray fluorescence and scanning X-ray diffraction microscopy at the Australian Synchrotron XFM beamline

    SciTech Connect

    Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.; Abbey, Brian; Vine, David J.; Nashed, Youssef S. G.; Mudie, Stephen T.; Afshar, Nader; Kirkham, Robin; Chen, Bo; Balaur, Eugeniu; de Jonge, Martin D.

    2016-08-11

    Owing to its extreme sensitivity, quantitative mapping of elemental distributionsviaX-ray fluorescence microscopy (XFM) has become a key microanalytical technique. The recent realisation of scanning X-ray diffraction microscopy (SXDM) meanwhile provides an avenue for quantitative super-resolved ultra-structural visualization. The similarity of their experimental geometries indicates excellent prospects for simultaneous acquisition. Here, in both step- and fly-scanning modes, robust, simultaneous XFM-SXDM is demonstrated.

  7. Apollo 15 Geochemical X-ray Fluorescence Experiment: Preliminary Report.

    PubMed

    Adler, I; Trombka, J; Gerard, J; Lowman, P; Schmadebeck, R; Blodget, H; Eller, E; Yin, L; Lamothe, R; Gorenstein, P; Bjorkholm, P

    1972-01-28

    Although only part of the information from the x-ray fluorescence geochemical experiment has been analyzed, it is clear that the experiment was highly successful. Significant compositional differences among and possibly within the maria and highlands have been detected. When viewed in the light of analyzed lunar rocks and soil samples, and the data from other lunar orbital experiments (in particular, the Apollo 15 gamma-ray spectroscopy experiment), the results indicate the existence of a differential lunar highland crust, probably feldspathic. This crust appears to be related to the plagioclase-rich materials previously found in the samples from Apollo 11, Apollo 12, Apollo 14, Apollo 15, and Luna 16.

  8. Portable X-ray Fluorescence Unit for Analyzing Crime Scenes

    NASA Astrophysics Data System (ADS)

    Visco, A.

    2003-12-01

    Goddard Space Flight Center and the National Institute of Justice have teamed up to apply NASA technology to the field of forensic science. NASA hardware that is under development for future planetary robotic missions, such as Mars exploration, is being engineered into a rugged, portable, non-destructive X-ray fluorescence system for identifying gunshot residue, blood, and semen at crime scenes. This project establishes the shielding requirements that will ensure that the exposure of a user to ionizing radiation is below the U.S. Nuclear Regulatory Commission's allowable limits, and also develops the benchtop model for testing the system in a controlled environment.

  9. Evaluating the variability of ceramics with x-ray fluorescence

    SciTech Connect

    Crown, P.L.; Schwalbe, L.A.; London, J.R.

    1984-01-01

    Our assessment of prehistoric trade in ceramics depends on our ability to identify and distinguish different sources of manufacture. For the American Southwest, archaeologists have proposed various models of ceramic manufacture and exchange. Until recently, conflicting hypotheses were tested mainly on the basis of petrographic analysis of nonplastic tempering materials. We have extended these analyses to include x-ray fluorescence (XRF). XRF provides a fast and inexpensive means of analyzing large numbers of samples. Since 1982, approximately 500 prehistoric sherds and 40 prepared clay and mineral samples have been examined with XRF. Multivariate statistical techniques have been applied to help identify groupings of samples with possible archaeological significance.

  10. Probing symmetry and symmetry breaking in resonant soft-x-ray fluorescence spectra of molecules

    SciTech Connect

    Glans, P.; Gunnelin, K.; Guo, J.

    1997-04-01

    Conventional non-resonant soft X-ray emission brings about information about electronic structure through its symmetry and polarization selectivity, the character of which is governed by simple dipole rules. For centro-symmetric molecules with the emitting atom at the inversion center these rules lead to selective emission through the required parity change. For the more common classes of molecules which have lower symmetry or for systems with degenerate core orbitals (delocalized over identical sites), it is merely the local symmetry selectivity that provides a probe of the local atomic orbital contribution to the molecular orbital. For instance, in X-ray spectra of first row species the intensities essentially map the p-density at each particular atomic site, and, in a molecular orbital picture, the contribution of the local p-type atomic orbitals in the LCAO description of the molecular orbitals. The situation is different for resonant X-ray fluorescence spectra. Here strict parity and symmetry selectivity gives rise to a strong frequency dependence for all molecules with an element of symmetry. In addition to symmetry selectivity the strong frequency dependence of resonant X-ray emission is caused by the interplay between the shape of a narrow X-ray excitation energy function and the lifetime and vibrational broadenings of the resonantly excited core states. This interplay leads to various observable effects, such as linear dispersion, resonance narrowing and emission line (Stokes) doubling. Also from the point of view of polarization selectivity, the resonantly excited X-ray spectra are much more informative than the corresponding non-resonant spectra. Examples are presented for nitrogen, oxygen, and carbon dioxide molecules.

  11. The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

    SciTech Connect

    Paterson, D.; Jonge, M. D. de; Howard, D. L.; Lewis, W.; McKinlay, J.; Starritt, A.; Kusel, M.; Ryan, C. G.; Kirkham, R.; Moorhead, G.; Siddons, D. P.

    2011-09-09

    A hard x-ray micro-nanoprobe has commenced operation at the Australian Synchrotron providing versatile x-ray fluorescence microscopy across an incident energy range from 4 to 25 keV. Two x-ray probes are used to collect {mu}-XRF and {mu}-XANES for elemental and chemical microanalysis: a Kirkpatrick-Baez mirror microprobe for micron resolution studies and a Fresnel zone plate nanoprobe capable of 60-nm resolution. Some unique aspects of the beamline design and operation are discussed. An advanced energy dispersive x-ray fluorescence detection scheme named Maia has been developed for the beamline, which enables ultrafast x-ray fluorescence microscopy.

  12. Preliminary Results on Studying of Meteorites from Geological Museum of Kazan University by X-Ray Fluorescence and Computed X-Ray Tomography

    NASA Astrophysics Data System (ADS)

    Kuzina, D. M.; Nurgaliev, D. K.; Gareev, B. I.; Batalin, G. A.; Silantev, V. V.; Statsenko, E. O.

    2017-02-01

    Micro X-ray fluorescence and X-ray computed tomography used for studying meteorites (particularly chondrules and iron-nickel alloys) from Geological Museum (Kazan), their elemental composition, and distribution of these objects in the body of meteorite.

  13. X-ray fluorescence surface contaminant analyzer: A feasibility study

    NASA Technical Reports Server (NTRS)

    Eldridge, Hudson B.

    1988-01-01

    The bonding of liner material to the inner metal surfaces of solid rocket booster cases is adversely affected by minute amounts of impurities on the metal surface. Suitable non-destructive methods currently used for detecting these surface contaminants do not provide the means of identifying their elemental composition. The feasibility of using isotopic source excited energy dispersive X-ray fluorescence as a possible technique for elemental analysis of such contaminants is investigated. A survey is made of the elemental compositions of both D-6ac steel, a common construction material for the booster cases, and Conoco HD-2 grease, a common surface contamination. Source and detector choices that maximize signal to noise ratio in a Recessed Source Geometry are made. A Monte Carlo simulation is then made of the optimized device incorporating the latest available X-ray constants at the energy of the chosen source to determine the device's response to a D-6ac steel surface contained with Conoco HD-2 grease.

  14. Development of suitable plastic standards for X-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Mans, Christian; Hanning, Stephanie; Simons, Christoph; Wegner, Anne; Janβen, Anton; Kreyenschmidt, Martin

    2007-02-01

    For the adoption of the EU directive "Restriction on use of certain Hazardous Substances" and "Waste Electrical and Electronic Equipment" using X-ray fluorescence analysis suitable standard materials are required. Plastic standards based on acrylonitrile-butadiene-styrene terpolymer, containing the regulated elements Br, Cd, Cr, Hg and Pb were developed and produced as granulates and solid bodies. The calibration materials were not generated as a dilution from one master batch but rather the element concentrations were distributed over nine independent calibration samples. This was necessary to enable inter-elemental corrections and empirical constant mass absorption coefficients. The produced standard materials are characterized by a homogenous element distribution, which is more than sufficient for X-ray fluorescence analysis. Concentrations for all elements except for Br could be determined by Inductively Coupled Plasma Atomic Emission Spectroscopy after microwave assisted digestion. The concentration of Br was determined by use of Neutron Activation Analysis at Hahn-Meitner-Institute in Berlin, Germany. The correlation of the X-ray fluorescence analysis measurements with the values determined using Inductively Coupled Plasma Atomic Emission Spectroscopy and Neutron Activation Analysis showed a very good linearity.

  15. Elemental analysis of waste glass by x-ray fluorescence spectrometry

    SciTech Connect

    Bickford, D.F.; Jurgensen, A.R.; Resce, J.L.; Ragsdale, R.G.; Overcamp, T.J.

    1995-05-01

    An X-ray fluorescence (XRF) technique is reported which shows promise for the elemental analysis of low-level mixed waste glasses. This technique can be used for both quantitative laboratory analysis and process control. The glass-forming melts are cast into graphite molds and resulting disks are annealed and polished. The disk is then analyzed with a wavelength dispersive X-ray fluorescence spectrometer and the elemental intensities are converted into concentration with a fundamental parameters routine without the use of matrix-matched standards. Precision of elemental determinations are all better than one percent relative standard deviation. The XRF analysis has been compared with a reference method utilizing conventional wet chemical dissolution techniques followed by atomic spectroscopic determination. Results show that there is no significant difference between these two techniques, however, the XRF technique is much simpler and faster than the wet chemical methods.

  16. Human thyroid specimen imaging by fluorescent x-ray computed tomography with synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Takeda, Tohoru; Yu, Quanwen; Yashiro, Toru; Yuasa, Tetsuya; Hasegawa, Yasuo; Itai, Yuji; Akatsuka, Takao

    1999-09-01

    Fluorescent x-ray computed tomography (FXCT) is being developed to detect non-radioactive contrast materials in living specimens. The FXCT system consists of a silicon (111) channel cut monochromator, an x-ray slit and a collimator for fluorescent x ray detection, a scanning table for the target organ and an x-ray detector for fluorescent x-ray and transmission x-ray. To reduce Compton scattering overlapped on the fluorescent K(alpha) line, incident monochromatic x-ray was set at 37 keV. The FXCT clearly imaged a human thyroid gland and iodine content was estimated quantitatively. In a case of hyperthyroidism, the two-dimensional distribution of iodine content was not uniform, and thyroid cancer had a small amount of iodine. FXCT can be used to detect iodine within thyroid gland quantitatively and to delineate its distribution.

  17. Determination of thorium by fluorescent x-ray spectrometry

    USGS Publications Warehouse

    Adler, I.; Axelrod, J.M.

    1955-01-01

    A fluorescent x-ray spectrographic method for the determination of thoria in rock samples uses thallium as an internal standard. Measurements are made with a two-channel spectrometer equipped with quartz (d = 1.817 A.) analyzing crystals. Particle-size effects are minimized by grinding the sample components with a mixture of silicon carbide and aluminum and then briquetting. Analyses of 17 samples showed that for the 16 samples containing over 0.7% thoria the average error, based on chemical results, is 4.7% and the maximum error, 9.5%. Because of limitations of instrumentation, 0.2% thoria is considered the lower limit of detection. An analysis can be made in about an hour.

  18. Counter tube window and X-ray fluorescence analyzer study

    NASA Technical Reports Server (NTRS)

    Hertel, R.; Holm, M.

    1973-01-01

    A study was performed to determine the best design tube window and X-ray fluorescence analyzer for quantitative analysis of Venusian dust and condensates. The principal objective of the project was to develop the best counter tube window geometry for the sensing element of the instrument. This included formulation of a mathematical model of the window and optimization of its parameters. The proposed detector and instrument has several important features. The instrument will perform a near real-time analysis of dust in the Venusian atmosphere, and is capable of measuring dust layers less than 1 micron thick. In addition, wide dynamic measurement range will be provided to compensate for extreme variations in count rates. An integral pulse-height analyzer and memory accumulate data and read out spectra for detail computer analysis on the ground.

  19. Using X-ray Fluorescence to Date Petroglyphs

    NASA Astrophysics Data System (ADS)

    McNeil, James

    2009-10-01

    Petroglyphs were created by ancient peoples of the Colorado Plateau who pecked figures of cultural or religious significance into the desert varnish, the ubiquitous dark patina covering the rock surfaces of the region. Manganese (Mn) is a significant elemental component of desert varnish that is often at trace levels in the substrate rock. As such, F. Lytle has shown that under certain conditions, it may be possible to estimate the age of petroglpyhs using Mn levels. In this work we use x-ray fluorescence to measure Mn levels in the desert varnish of petroglyphs and then use dated graffiti to attempt to calibrate the Mn level with age. Preliminary results from petroglyph panels in eastern Utah will be presented.

  20. X-Ray Fluorescence Microscopy for Investigation of Archival Tissues

    PubMed Central

    Paunesku, T.; Wanzer, M. B.; Kirillova, E. N.; Muksinova, K. N.; Revina, V. S.; Romanov, S. A.; Lyubchansky, E. R.; Grosche, B.; Birschwilks, M.; Vogt, S.; Finney, L.; Woloschak, G. E.

    2013-01-01

    Several recent efforts in radiation biology community worldwide have amassed records and archival tissues from animals exposed to different radionuclides and external beam irradiation. In most cases, these samples come from life-long studies on large animal populations conducted in national laboratories and equivalent institutions throughout Europe, North America, and Japan. While many of these tissues were used for histopathological analyses, much more information may still be obtained from these samples. A new technique suitable for imaging of these tissues is X-Ray Fluorescence Microscopy (XFM). Following development of third generation synchrotrons, XFM has emerged as an ideal technique for study of metal content, speciation, and localization in cells, tissues and organs. Here we review some of the recent XFM literature pertinent to tissue sample studies and present examples of XFM data obtained from tissue sections of beagle dog samples which show that the quality of archival tissues allows XFM investigation. PMID:22951477

  1. Comparison of the data of X-ray microtomography and fluorescence analysis in the study of bone-tissue structure

    NASA Astrophysics Data System (ADS)

    Asadchikov, V. E.; Senin, R. A.; Blagov, A. E.; Buzmakov, A. V.; Gulimova, V. I.; Zolotov, D. A.; Orekhov, A. S.; Osadchaya, A. S.; Podurets, K. M.; Savel'ev, S. V.; Seregin, A. Yu.; Tereshchenko, E. Yu.; Chukalina, M. V.; Kovalchuk, M. V.

    2012-09-01

    The possibility of localizing clusters of heavy atoms is substantiated by comparing the data of X-ray microtomography at different wavelengths, scanning electron microscopy, and X-ray fluorescence analysis. The proximal tail vertebrae of Turner's thick-toed gecko ( Chondrodactylus turneri) have been investigated for the first time by both histological and physical methods, including X-ray microtomography at different wavelengths and elemental analysis. This complex methodology of study made it possible to reveal the regions of accumulation of heavy elements in the aforementioned bones of Turner's thick-toed gecko.

  2. Comparative studies of X-ray images and fluorescence images of the same specimens

    NASA Astrophysics Data System (ADS)

    Majima, T.; Tomie, T.; Shimizu, H.

    2003-03-01

    A flash contact soft x-ray microscope using laser-induced plasma as a flash x-ray source is a practical instrument for observation of living organisms in water [1-4]. As previously reported we developed a tabletop flash contact soft x-ray microscope System [3]. In this System, x-ray images are given as whole projection of the specimens on the PMMA membrane. This causes us some complexity for understanding the x-ray images. It is necessary to attribute features in the x-ray images to sub-cellular structures of the specimen. For this purpose we have developed a new sample holder, where specimens are observable with a fluorescence microscope just before x-ray exposure. Fluorescence images of onion epidermal cells stained by DAPI and x-ray images of the same specimens are compared.

  3. X-Ray fluorescence analysis of trace elements in fruit juice

    NASA Astrophysics Data System (ADS)

    Bao, Sheng-Xiang; Wang, Zhi-Hong; Liu, Jing-Song

    1999-12-01

    X-Ray fluorescence spectrometry is applied to the determination of trace elements in fruit juice characterized by a high content of sugar and other soluble solid substances. Samples are prepared by evaporation, carbonization and pressing into discs. The synthesis of standards is described in detail. All element concentrations are directly estimated from linear calibration curves obtained without any matrix correction. The results of the analysis are in good agreement with those given by inductively coupled plasma-atomic emission spectrometry and atomic absorption spectrometry techniques.

  4. Depth-Resolved X-ray Absorption Spectroscopy by Means of Grazing Emission X-ray Fluorescence.

    PubMed

    Kayser, Yves; Sá, Jacinto; Szlachetko, Jakub

    2015-11-03

    Grazing emission X-ray fluorescence (GEXRF) is well suited for nondestructive elemental-sensitive depth-profiling measurements on samples with nanometer-sized features. By varying the grazing emission angle under which the X-ray fluorescence signal is detected, the probed depth range can be tuned from a few to several hundred nanometers. The dependence of the XRF intensity on the grazing emission angle can be assessed in a sequence of measurements or in a scanning-free approach using a position-sensitive area detector. Hereafter, we will show that the combination of scanning-free GEXRF and fluorescence detected X-ray absorption spectroscopy (XAS) allows for depth-resolved chemical speciation measurements with nanometer-scale accuracy. While the conventional grazing emission geometry is advantageous to minimize self-absorption effects, the use of a scanning-free setup makes the sequential scanning of the grazing emission angles obsolete and paves the way toward time-resolved depth-sensitive XAS measurements. The presented experimental approach was applied to study the surface oxidation of an Fe layer on the top of bulk Si and of a Ge bulk sample. Thanks to the penetrating properties and the insensitivity toward the electric conduction properties of the incident and emitted X-rays, the presented experimental approach is well suited for in situ sample surface studies in the nanometer regime.

  5. Total reflection x-ray fluorescence: Determination of an optimum geometry

    SciTech Connect

    Koo, Y.M.; Chang, C.H.; Padmore, H.A.

    1997-04-01

    Total reflection X-Ray Fluorescence (TXRF) is a widely used technique in which the normal trace element detection capability of hard x-ray fluorescence (XRF) is enhanced by use of an x-ray reflective substrate. TXRF is more sensitive than normal photon induced XRF due to the reduction of the substrate scattering and fluorescence signals. This reduction comes about because in total external reflection, the photon field only penetrates about 20 {angstrom} into the surface, instead of typically 50 {mu}m for a silicon substrate at normal incidence for 10 KeV photons. The technique is used in many fields of trace element analysis, and is widely used in the determination of metal impurity concentrations on and in the surface of silicon wafers. The Semiconductor Industry Association roadmap (SIA) indicates a need for wafer contamination detection at the 10{sup 7}atoms/cm{sup 2} level in the next few years. Current commercial systems using rotating anode x-ray sources presently routinely operate with a sensitivity level of around 10{sup 10} atoms/cm{sup 2} and this has led to interest in the use of synchrotron radiation to extend the sensitivity by three orders of magnitude. The pioneering work of Pianetta and co-workers at SSRL has clearly shown that this should be possible, using a fully optimized source and detector. The purpose of this work is to determine whether ALS would be a suitable source for this type of highly sensitive wafer TXRF. At first look it appears improbable as the SSRL work used a high flux multipole wiggler source, and it is clear that the detected fluorescence for relevant concentrations is small. In addition, SSRL operates at 3.0 GeV rather than 1.9 GeV, and is therefore more naturally suited to hard x-ray experiments. The aim of this work was therefore to establish a theoretical model for the scattering and fluorescence processes, so that one could predict the differences between alternative geometries and select an optimum configuration.

  6. In Vivo X-Ray Fluorescence Microtomographic Imaging of Elements in Single-Celled Fern Spores

    SciTech Connect

    Hirai, Yasuharu; Yoneyama, Akio; Hisada, Akiko; Uchida, Kenko

    2007-01-19

    We have observed in vivo three-dimensional distributions of constituent elements of single-celled spores of the fern Adiantum capillus-veneris using an X-ray fluorescence computed microtomography method. The images of these distributions are generated from a series of slice data, each of which is acquired by a sample translation-rotation method. An incident X-ray microbeam irradiates the sample with a spot size of 1 {mu}m. The high Ca concentration in the testa and the localized and overlapping Fe and Zn concentrations inside the spore are shown in three-dimensional images. The K concentration is high throughout the cell, and there are localized regions of higher density. The atomic number densities of these elements in the testa and inside the cell in a tomographic slice are estimated with a resolution of about 1 {mu}m.

  7. Flow method and apparatus for screening chemicals using micro x-ray fluorescence

    DOEpatents

    Warner, Benjamin P.; Havrilla, George J.; Miller, Thomasin C.; Lewis, Cris; Mahan, Cynthia A.; Wells, Cyndi A.

    2009-04-14

    Method and apparatus for screening chemicals using micro x-ray fluorescence. A method for screening a mixture of potential pharmaceutical chemicals for binding to at least one target binder involves flow-separating a solution of chemicals and target binders into separated components, exposing them to an x-ray excitation beam, detecting x-ray fluorescence signals from the components, and determining from the signals whether or not a binding event between a chemical and target binder has occurred.

  8. Flow method and apparatus for screening chemicals using micro x-ray fluorescence

    DOEpatents

    Warner, Benjamin P [Los Alamos, NM; Havrilla, George J [Los Alamos, NM; Miller, Thomasin C [Bartlesville, OK; Lewis, Cris [Los Alamos, NM; Mahan, Cynthia A [Los Alamos, NM; Wells, Cyndi A [Los Alamos, NM

    2011-04-26

    Method and apparatus for screening chemicals using micro x-ray fluorescence. A method for screening a mixture of potential pharmaceutical chemicals for binding to at least one target binder involves flow separating a solution of chemicals and target binders into separated components, exposing them to an x-ray excitation beam, detecting x-ray fluorescence signals from the components, and determining from the signals whether or not a binding event between a chemical and target binder has occurred.

  9. Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil.

    PubMed

    Kappen, P; Arhatari, B D; Luu, M B; Balaur, E; Caradoc-Davies, T

    2013-06-01

    This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography∕diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

  10. Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil

    NASA Astrophysics Data System (ADS)

    Kappen, P.; Arhatari, B. D.; Luu, M. B.; Balaur, E.; Caradoc-Davies, T.

    2013-06-01

    This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography/diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

  11. A Comprehensive X-Ray Absorption Model for Atomic Oxygen

    NASA Technical Reports Server (NTRS)

    Gorczyca, T. W.; Bautista, M. A.; Hasoglu, M. F.; Garcia, J.; Gatuzz, E.; Kaastra, J. S.; Kallman, T. R.; Manson, S. T.; Mendoza, C.; Raassen, A. J. J.; de Vries, C. P.; Zatsarinny, O.

    2013-01-01

    An analytical formula is developed to accurately represent the photoabsorption cross section of atomic Oxygen for all energies of interest in X-ray spectral modeling. In the vicinity of the K edge, a Rydberg series expression is used to fit R-matrix results, including important orbital relaxation effects, that accurately predict the absorption oscillator strengths below threshold and merge consistently and continuously to the above-threshold cross section. Further, minor adjustments are made to the threshold energies in order to reliably align the atomic Rydberg resonances after consideration of both experimental and observed line positions. At energies far below or above the K-edge region, the formulation is based on both outer- and inner-shell direct photoionization, including significant shake-up and shake-off processes that result in photoionization-excitation and double-photoionization contributions to the total cross section. The ultimate purpose for developing a definitive model for oxygen absorption is to resolve standing discrepancies between the astronomically observed and laboratory-measured line positions, and between the inferred atomic and molecular oxygen abundances in the interstellar medium from XSTAR and SPEX spectral models.

  12. ITER core imaging X-ray spectroscopy: Atomic physics issues

    NASA Astrophysics Data System (ADS)

    Beiersdorfer, P.; Clementson, J.; Widmann, K.; Bitter, M.; Hill, K. W.; Johnson, D.; Barnsley, R.; Chung, H. K.; Safronova, U. I.

    2017-03-01

    The Core Imaging X-Ray Spectrometer (CIXS) will be employed for measurements of the ion temperature and of the toroidal rotation velocity, Ti and vϕ, respectively, as a function of the radius of ITER plasmas. The diagnostic is based on precision determinations of the Doppler broadening, centroid shift, and intensity of the lines of highly ionized heavy impurities using a curved Bragg crystal spectral disperser and imager. The ions under consideration for the diagnostic are those of tungsten, krypton, xenon, iron, and argon. A detailed discussion is given of the need for atomic physics experiments and calculations involving the primary diagnostic lines and their collisional and dielectronic satellites. Such experiments and calculations define the instrument parameters, determine the diagnostic uncertainties, and provide paths for extending the diagnostic capabilities to measure impurity concentrations, electron temperature, and ion transport parameters. Enabling the diagnostic to measure radially dependent ion transport coefficients, in particular, requires a large amount of high-quality atomic data in the form of reliable excitation, ionization, and recombination rate coefficients as well as ionization balance calculations which make use of these data. Because core imaging spectrometers are being developed and implemented on present-day magnetic fusion devices, much of the atomic data are already needed and can be tested in the analysis of existing spectra recorded by these diagnostics.

  13. X-ray Fluorescence Measurements of Turbulent Methane-Oxygen Shear Coaxial Flames

    DTIC Science & Technology

    2015-05-01

    number of positive attributes of x-ray fluorescence physics, particularly insensitivity to chemical bonding (which results in tracers being conserved... rocket engines where, due to the high temperature, it is difficult to obtain quantitative mixing field measurements using conventional optical...temperature flames is attractive due to a number of positive attributes of x-ray fluorescence physics, particularly insensitivity to chemical bonding

  14. Dual x-ray fluorescence spectrometer and method for fluid analysis

    DOEpatents

    Wilson, Bary W.; Shepard, Chester L.

    2005-02-22

    Disclosed are an X-ray fluorescence (SRF) spectrometer and method for on-site and in-line determination of contaminant elements in lubricating oils and in fuel oils on board a marine vessel. An XRF source block 13 contains two radionuclide sources 16, 17 (e.g. Cd 109 and Fe 55), each oriented 180 degrees from the other to excite separate targets. The Cd 109 source 16 excites sample lube oil flowing through a low molecular weight sample line 18. The Fe 55 source 17 excites fuel oil manually presented to the source beam inside a low molecular weight vial 26 or other container. Two separate detectors A and B are arranged to detect the fluorescent x-rays from the targets, photons from the analyte atoms in the lube oil for example, and sulfur identifying x-rays from bunker fuel oil for example. The system allows both automated in-line and manual on-site analysis using one set of signal processing and multi-channel analyzer electronics 34, 37 as well as one computer 39 and user interface 43.

  15. Measurement of plutonium in spent nuclear fuel by self-induced x-ray fluorescence

    SciTech Connect

    Hoover, Andrew S; Rudy, Cliff R; Tobin, Steve J; Charlton, William S; Stafford, A; Strohmeyer, D; Saavadra, S

    2009-01-01

    Direct measurement of the plutonium content in spent nuclear fuel is a challenging problem in non-destructive assay. The very high gamma-ray flux from fission product isotopes overwhelms the weaker gamma-ray emissions from plutonium and uranium, making passive gamma-ray measurements impossible. However, the intense fission product radiation is effective at exciting plutonium and uranium atoms, resulting in subsequent fluorescence X-ray emission. K-shell X-rays in the 100 keV energy range can escape the fuel and cladding, providing a direct signal from uranium and plutonium that can be measured with a standard germanium detector. The measured plutonium to uranium elemental ratio can be used to compute the plutonium content of the fuel. The technique can potentially provide a passive, non-destructive assay tool for determining plutonium content in spent fuel. In this paper, we discuss recent non-destructive measurements of plutonium X-ray fluorescence (XRF) signatures from pressurized water reactor spent fuel rods. We also discuss how emerging new technologies, like very high energy resolution microcalorimeter detectors, might be applied to XRF measurements.

  16. Bone lead measured by X-ray fluorescence: epidemiologic methods.

    PubMed Central

    Hu, H; Aro, A; Rotnitzky, A

    1995-01-01

    In vivo X-ray fluorescence (XRF) measurement of bone lead concentration (XRF) has emerged as an important technique for future epidemiological studies of long-term toxicity. Several issues germane to epidemiologic methodology need to be addressed, however. First, sources of variability in measurements of bone lead need to be quantified, including imprecision related to the physical measurement itself and the variability of lead deposition over the two main compartments of bones (cortical vs. trabecular) and within each compartment. Imprecision related to the physical measurement can be estimated for each individual measurement based on the variability of the signal and background. Second, approaches to low-level data need to be debated. We argue for using the minimal detection limit (MDL) to compare instruments and interpret individual measurements; however, with regard to epidemiologic studies, we would abandon the MDL in favor of using all point estimates. In analyses using bone lead as an independent variable, statistical techniques can be used to adjust regression estimates based on estimates of measurement uncertainty and bone lead variability. Third, factors that can be expected to modify the relationship between bone lead and toxicity such as gravida history, endocrinological states, nutrition, and other important influences on bone metabolism, need to be identified and measured in epidemiologic studies. By addressing these issues, investigators will be able to maximize the utility of XRF measurements in environmental epidemiologic studies. Images Figure 2. PMID:7621788

  17. Portable x-ray fluorescence spectrometer. Innovative technology summary report

    SciTech Connect

    1998-12-01

    This report describes the application of portable X-ray fluorescence (XRF) spectrometry to characterize materials related to deactivation and decommissioning (D and D) of contaminated facilities. Two portable XRF instruments manufactured by TN Spectrace were used in a technology evaluation as part of the Large-Scale Demonstration Project (LSDP) held at the Chicago Pile-5 Research Reactor (CP-5) located at Argonne National Laboratory (ANL). The LSDP is sponsored by the US Department of Energy (DOE), Office of Science and Technology, Deactivation and Decommissioning Focus Are (DDFA). The objective of the LSDP is to demonstrate innovative technologies or technology applications potentially beneficial to the D and D of contaminated facilities. The portable XRF technology offers several potential benefits for rapid characterization of facility components and contaminants, including significant cost reduction, fast turnaround time,a nd virtually no secondary waste. Field work for the demonstration of the portable XRF technology was performed from August 28--September 3, 1996 and October 30--December 13, 1996.

  18. High-throughput screening with micro-x-ray fluorescence

    SciTech Connect

    Havrilla, George J.; Miller, Thomasin C.

    2005-06-15

    Micro-x-ray fluorescence (MXRF) is a useful characterization tool for high-throughput screening of combinatorial libraries. Due to the increasing threat of use of chemical warfare (CW) agents both in military actions and against civilians by terrorist extremists, there is a strong push to improve existing methods and develop means for the detection of a broad spectrum of CW agents in a minimal amount of time to increase national security. This paper describes a combinatorial high-throughput screening technique for CW receptor discovery to aid in sensor development. MXRF can screen materials for elemental composition at the mesoscale level (tens to hundreds of micrometers). The key aspect of this work is the use of commercial MXRF instrumentation coupled with the inherent heteroatom elements within the target molecules of the combinatorial reaction to provide rapid and specific identification of lead species. The method is demonstrated by screening an 11-mer oligopeptide library for selective binding of the degradation products of the nerve agent VX. The identified oligopeptides can be used as selective molecular receptors for sensor development. The MXRF screening method is nondestructive, requires minimal sample preparation or special tags for analysis, and the screening time depends on the desired sensitivity.

  19. High-throughput screening with micro-x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Havrilla, George J.; Miller, Thomasin C.

    2005-06-01

    Micro-x-ray fluorescence (MXRF) is a useful characterization tool for high-throughput screening of combinatorial libraries. Due to the increasing threat of use of chemical warfare (CW) agents both in military actions and against civilians by terrorist extremists, there is a strong push to improve existing methods and develop means for the detection of a broad spectrum of CW agents in a minimal amount of time to increase national security. This paper describes a combinatorial high-throughput screening technique for CW receptor discovery to aid in sensor development. MXRF can screen materials for elemental composition at the mesoscale level (tens to hundreds of micrometers). The key aspect of this work is the use of commercial MXRF instrumentation coupled with the inherent heteroatom elements within the target molecules of the combinatorial reaction to provide rapid and specific identification of lead species. The method is demonstrated by screening an 11-mer oligopeptide library for selective binding of the degradation products of the nerve agent VX. The identified oligopeptides can be used as selective molecular receptors for sensor development. The MXRF screening method is nondestructive, requires minimal sample preparation or special tags for analysis, and the screening time depends on the desired sensitivity.

  20. In vivo X-ray fluorescence of lead in bone

    SciTech Connect

    Todd, A.C.; McNeill, F.E.; Fowler, B.A. )

    1992-12-01

    The in vivo measurement of lead in bone by K X-ray fluorescence (K XRF) is becoming an increasingly widely utilized technique for assessing long-term lead dosimetry. Several groups have already reported the development of in vivo measurement systems, the majority adopting the [sup 109]Cd/backscatter K XRF technique because of its substantial advantages in terms of a robust measurement, lower detection limit (compared with [sup 57]Co/90[degrees]), absence of the need for sedation of younger subjects, and lower effective (radiation) dose when alculated according to the most recent guidelines. The advantages of the [sup 109]Cd system are primarily a consequence of the physics principles of the technique. The apparatus of each XRF technique is transportable, facilitating easy establishment of mobile laboratory facilities. More research is needed to substantiate claims made for particular XRF technologies, but both L and K XRF techniques provide the possibility of improved understanding of the body's handling of the ubiquitious toxin lead. 44 refs., 2 figs., 1 tab.

  1. X-Ray Fluorescence Spectrometric Analysis of Wear Metals in used Lubricating Oils.

    DTIC Science & Technology

    1980-12-01

    34Sea King". On a comparg les valeurs obtenues A l’aide de cette uithode avec celles obtenues par absorption atomique aur des 6chantillons...contaminantes et permettraient de d~celer plus t8t que l’analyse par absorption atomique une usure anormale d’apras le changement plus marqug des quantit~s de...ray fluorescence wear metal levels were compared to the atomic absorption wear metal levels determined on corresponding samples. In general, the x-ray

  2. Spectrometric determination of chromium in FD&C blue no. 1 by X-ray fluorescence.

    PubMed

    Hepp, N M

    1996-01-01

    An X-ray fluorescence spectrometry (XRF) method was developed and validated for determination of chromium in FD&C Blue No. 1. Results of this analysis were compared with those obtained with an atomic absorption spectroscopy (AAS) method currently used by the U.S. Food and Drug Administration. Levels of Cr, as determined by the XRF and AAS methods, were comparable. The limit of quantitation for the XRF method is 4 micrograms Cr/g. The predicted 95% confidence interval at the specification level is 50 +/- 5 micrograms/g.

  3. A comprehensive X-ray absorption model for atomic oxygen

    SciTech Connect

    Gorczyca, T. W.; Bautista, M. A.; Mendoza, C.; Hasoglu, M. F.; García, J.; Gatuzz, E.; Kaastra, J. S.; Raassen, A. J. J.; De Vries, C. P.; Kallman, T. R.; Manson, S. T.; Zatsarinny, O.

    2013-12-10

    An analytical formula is developed to accurately represent the photoabsorption cross section of O I for all energies of interest in X-ray spectral modeling. In the vicinity of the K edge, a Rydberg series expression is used to fit R-matrix results, including important orbital relaxation effects, that accurately predict the absorption oscillator strengths below threshold and merge consistently and continuously to the above-threshold cross section. Further, minor adjustments are made to the threshold energies in order to reliably align the atomic Rydberg resonances after consideration of both experimental and observed line positions. At energies far below or above the K-edge region, the formulation is based on both outer- and inner-shell direct photoionization, including significant shake-up and shake-off processes that result in photoionization-excitation and double-photoionization contributions to the total cross section. The ultimate purpose for developing a definitive model for oxygen absorption is to resolve standing discrepancies between the astronomically observed and laboratory-measured line positions, and between the inferred atomic and molecular oxygen abundances in the interstellar medium from XSTAR and SPEX spectral models.

  4. Gold nanoclusters as contrast agents for fluorescent and X-ray dual-modality imaging.

    PubMed

    Zhang, Aili; Tu, Yu; Qin, Songbing; Li, Yan; Zhou, Juying; Chen, Na; Lu, Qiang; Zhang, Bingbo

    2012-04-15

    Multimodal imaging technique is an alternative approach to improve sensitivity of early cancer diagnosis. In this study, highly fluorescent and strong X-ray absorption coefficient gold nanoclusters (Au NCs) are synthesized as dual-modality imaging contrast agents (CAs) for fluorescent and X-ray dual-modality imaging. The experimental results show that the as-prepared Au NCs are well constructed with ultrasmall sizes, reliable fluorescent emission, high computed tomography (CT) value and fine biocompatibility. In vivo imaging results indicate that the obtained Au NCs are capable of fluorescent and X-ray enhanced imaging.

  5. X-ray fluorescence spectrometry of the Moon by the XRS onboard SELENE-Kaguya

    NASA Astrophysics Data System (ADS)

    Okada, Tatsuaki; Shiraishi, Hiroaki; Kato, Manabu; Grande, Manuel; Shirai, Kei; Yamamoto, Yukio; Arai, Takehiko; Ogawa, Kazunori

    The X-ray fluorescence spectrometer (XRS) onboard SELENE-Kaguya is now observing the Moon from the lunar polar circular orbit at about 100km altitude. The XRS aims at an investigation of lunar major elemental composition by remote X-ray fluorescence method. Solar X-rays enter into the lunar surface and excite X-rays characteristic of each element in the uppermost several tens of micrometer of the lunar surface. Concurrent measurements of X- rays from the Moon and the Sun allow quantitative elemental analysis of lunar surface. The XRS is a charge-coupled device based X-ray spectrometer, using the heritage technology of the instrument onboard Hayabusa, which rendezvoused and observed asteroid 25143 Itokawa. This study will report the latest results of the XRS observations, though it is now suffering from low signal to background ratios due to the very faint solar activity in recent several months.

  6. Energy response calibration of photon-counting detectors using X-ray fluorescence: a feasibility study

    PubMed Central

    Cho, H-M; Ding, H; Ziemer, BP; Molloi, S

    2014-01-01

    Accurate energy calibration is critical for the application of energy-resolved photon-counting detectors in spectral imaging. The aim of this study is to investigate the feasibility of energy response calibration and characterization of a photon-counting detector using X-ray fluorescence. A comprehensive Monte Carlo simulation study was performed using Geant4 Application for Tomographic Emission (GATE) to investigate the optimal technique for X-ray fluorescence calibration. Simulations were conducted using a 100 kVp tungsten-anode spectra with 2.7 mm Al filter for a single pixel cadmium telluride (CdTe) detector with 3 × 3 mm2 in detection area. The angular dependence of X-ray fluorescence and scatter background was investigated by varying the detection angle from 20° to 170° with respect to the beam direction. The effects of the detector material, shape, and size on the recorded X-ray fluorescence were investigated. The fluorescent material size effect was considered with and without the container for the fluorescent material. In order to provide validation for the simulation result, the angular dependence of X-ray fluorescence from five fluorescent materials was experimentally measured using a spectrometer. Finally, eleven of the fluorescent materials were used for energy calibration of a CZT-based photon-counting detector. The optimal detection angle was determined to be approximately at 120° with respect to the beam direction, which showed the highest fluorescence to scatter ratio (FSR) with a weak dependence on the fluorescent material size. The feasibility of X-ray fluorescence for energy calibration of photon-counting detectors in the diagnostic X-ray energy range was verified by successfully calibrating the energy response of a CZT-based photon-counting detector. The results of this study can be used as a guideline to implement the X-ray fluorescence calibration method for photon-counting detectors in a typical imaging laboratory. PMID:25369288

  7. Determination of the implantation dose in silicon wafers by X-ray fluorescence analysis

    SciTech Connect

    Klockenkaemper, R.; Becker, M.; Bubert, H.; Burba, P. ); Palmetshofer, L. )

    1990-08-01

    The ion dose implanted in silicon wafers was determined by X-ray fluorescence analysis after the implantation process. As only near-surface layers below 1-{mu}m thickness were considered, the calibration could be carried out with external standards consisting of thin films of doped gelatine spread on pure wafers. Dose values for Cr and Co were determined between 4 {times} 10{sup 15} and 2 {times} 10{sup 17} atoms/cm{sup 2}, the detection limits being about 3 {times} 10{sup 14} atoms/cm{sup 2}. The results are precise and accurate apart from a residual scatter of less than 7%. This was confirmed by flame atomic absorption spectrometry after volatilization of the silicon matrix as SiF{sub 4}. It was found that ion-current measurements carried out during the implantation process can have considerable systematic errors.

  8. The fluorescence-dominated X-ray spectrum of the spiral galaxy NGC 6552

    NASA Technical Reports Server (NTRS)

    Fukazawa, Yasushi; Makishima, Kazuo; Ebisawa, Ken; Fabian, Andrew C.; Gendreau, Keith C.; Ikebe, Yasushi; Iwasawa, Kazushi; Kii, Tsuneo; Mushotzky, Richard F.; Ohashi, Takaya

    1994-01-01

    A hard X-ray source with a 2-10 keV flux of approximately 6 x 10(exp -13) ergs/sec/sq cm was detected with ASCA in the north ecliptic pole region. It is identified with the spiral galaxy NGC 6552 at a redshift of z = 0.026, which is optically classified as a Seyfert 2 galaxy. The X-ray spectrum consists of a series of atomic K-emission lines from (nearly-) neutral species of at least seven abundant elements, and a heavily absorbed (N(sub H) approx. = 6 x 10(exp 23)/sq cm) hard continuum. The iron line has an equivalent width as large as approximately 0.9 keV. Our results show that NGC 6552 is an extreme type 2 Seyfert galaxy, in which the fluorescent lines are produced when hard X-rays from a hidden active nucleus are reflected off thick cool matter into our line of sight. The intrinsic 2-10 keV luminosity of the nucleus is estimated to be at least 6 x 10(exp 42) ergs/s.

  9. Spectral Interferences Manganese (Mn) - Europium (Eu) Lines in X-Ray Fluorescence Spectrometry Spectrum

    NASA Astrophysics Data System (ADS)

    Tanc, Beril; Kaya, Mustafa; Gumus, Lokman; Kumral, Mustafa

    2016-04-01

    X-ray fluorescence (XRF) spectrometry is widely used for quantitative and semi quantitative analysis of many major, minor and trace elements in geological samples. Some advantages of the XRF method are; non-destructive sample preparation, applicability for powder, solid, paste and liquid samples and simple spectrum that are independent from chemical state. On the other hand, there are some disadvantages of the XRF methods such as poor sensitivity for low atomic number elements, matrix effect (physical matrix effects, such as fine versus course grain materials, may impact XRF performance) and interference effect (the spectral lines of elements may overlap distorting results for one or more elements). Especially, spectral interferences are very significant factors for accurate results. In this study, semi-quantitative analyzed manganese (II) oxide (MnO, 99.99%) was examined. Samples were pelleted and analyzed with XRF spectrometry (Bruker S8 Tiger). Unexpected peaks were obtained at the side of the major Mn peaks. Although sample does not contain Eu element, in results 0,3% Eu2O3 was observed. These result can occur high concentration of MnO and proximity of Mn and Eu lines. It can be eliminated by using correction equation or Mn concentration can confirm with other methods (such as Atomic absorption spectroscopy). Keywords: Spectral Interferences; Manganese (Mn); Europium (Eu); X-Ray Fluorescence Spectrometry Spectrum.

  10. X-ray fluorescence analyzers for investigating postmediaeval pottery from Southern Moravia.

    PubMed

    Trojek, Tomás; Hlozek, Matin; Cechák, Tomás; Musílek, Ladislav

    2010-01-01

    This paper deals with an investigation of ceramic archaeological finds with the use of in-situ X-ray fluorescence analysis. Firstly, three configurations of X-ray fluorescence analyzers constructed and used at the Czech Technical University in Prague are described and compared for use in a non-destructive survey of siliceous materials. Detection limits, depth of analysis, the relation of the analyzed area, the homogeneity of the samples, and variations in the element concentrations are discussed. Secondly, many shards of postmediaeval pottery from Southern Moravia are analyzed with X-ray fluorescence analysis and some of them also with electron microprobe analysis. Selected results are described.

  11. Some radiation effects on organic binders in X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Novosel-Radović, Vj.; MaljkoviĆ, Da.; NenadiĆ, N.

    The paper deals with diminished wear resistance of standard samples in X-ray fluorescence spectrometry. The effect of X-ray irradiation on pellet samples, pressed with starch as organic binder, was investigated by sieve analysis and scanning electron microscopy. A change in the starch grain size was found as a result of swelling and cracking.

  12. Application of confocal X-ray fluorescence micro-spectroscopy to the investigation of paint layers.

    PubMed

    Sun, Tianxi; Liu, Zhiguo; Wang, Guangfu; Ma, Yongzhong; Peng, Song; Sun, Weiyuan; Li, Fangzuo; Sun, Xuepeng; Ding, Xunliang

    2014-12-01

    A confocal micro X-ray fluorescence (MXRF) spectrometer based on polycapillary X-ray optics was used for the identification of paint layers. The performance of the confocal MXRF was studied. Multilayered paint fragments of a car were analyzed nondestructively to demonstrate that this confocal MXRF instrument could be used in the discrimination of the various layers in multilayer paint systems.

  13. Laboratory-based micro-X-ray fluorescence setup using a von Hamos crystal spectrometer and a focused beam X-ray tube.

    PubMed

    Kayser, Y; Błachucki, W; Dousse, J-Cl; Hoszowska, J; Neff, M; Romano, V

    2014-04-01

    The high-resolution von Hamos bent crystal spectrometer of the University of Fribourg was upgraded with a focused X-ray beam source with the aim of performing micro-sized X-ray fluorescence (XRF) measurements in the laboratory. The focused X-ray beam source integrates a collimating optics mounted on a low-power micro-spot X-ray tube and a focusing polycapillary half-lens placed in front of the sample. The performances of the setup were probed in terms of spatial and energy resolution. In particular, the fluorescence intensity and energy resolution of the von Hamos spectrometer equipped with the novel micro-focused X-ray source and a standard high-power water-cooled X-ray tube were compared. The XRF analysis capability of the new setup was assessed by measuring the dopant distribution within the core of Er-doped SiO2 optical fibers.

  14. Characterization of a pulsed x-ray source for fluorescent lifetime measurements

    NASA Astrophysics Data System (ADS)

    Blankespoor, S. C.; Derenzo, S. E.; Moses, W. W.; Rossington, C. S.; Ito, M.; Oba, K.

    1994-08-01

    To search for new, fast, inorganic scintillators, we have developed a bench-top pulsed x-ray source for determining fluorescent lifetimes and wavelengths of compounds in crystal or powdered form. This source uses a light-excited x-ray tube which produces x-rays when light from a laser diode strikes its photocathode. The x-ray tube has a tungsten anode, a beryllium exit window, a 30 kV maximum tube bias, and a 50 mu A maximum average cathode current. The laser produces 3 x 10(sup 7) photons at 650 nm per approximately 100 ps pulse, with up to 10(sup 7) pulses/sec. The time spread for the laser diode, x-ray tube, and a microchannel plate photomultiplier tube is less than 120 ps fwhm. The mean x-ray energy at tube biases of 20, 25, and 30 kV is 9.4, 10.3, and 11.1 keV, respectively. We measured 140, 230, and 330 x-ray photons per laser diode pulse per steradian, at tube biases of 20, 25, and 30 kV, respectively. Background x-rays due to dark current occur at a rate of 1 x 10(sup 6) and 3 x 10(sup 6) photons/sec/steradian at biases of 25 and 30 kV, respectively. Data characterizing the x-ray output with an aluminum filter in the x-ray beam are also presented.

  15. Site-specific distribution of copper, selenium, and zinc in human kidney by synchrotron radiation induced X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Homma, Shino; Nakai, Izumi; Misawa, Syogo; Shimojo, Nobuhiro

    1995-10-01

    Distribution of trace elements such as Cu, Se, and Zn in human kidney was examined by use of nondestructive synchrotron radiation X-ray fluorescence (SR-XRF) imaging technique. All elements measured were more accumulated in the renal cortex than in the medulla. The renal Cu and Zn distributions obtained by SR-XRF imaging were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). Furthermore, correlation analysis based on the X-ray intensity data of each analytical point showed a positive correlation of the distribution of these elements.

  16. X-ray fluorescence analysis of wear metals in used lubricating oils

    NASA Technical Reports Server (NTRS)

    Maddox, W. E.; Kelliher, W. C.

    1986-01-01

    Used oils from several aircraft at NASA's Langley Research Center were analyzed over a three year period using X-ray fluorescence (XRF) and atomic emission spectrometry. The results of both analyses are presented and comparisons are made. Fe and Cu data for oil from four internal combustion engines are provided and XRF and atomic emission spectrometry measurements were found to be in perfect agreement. However, distributions were found in the case of oil from a jet aircraft engine whereby the latter method gave values for total iron concentration in the oil and did not distinguish between suspended particles and oil additives. XRF does not have these particle-size limitations; moreover, it is a faster process. It is concluded that XRF is the preferred method in the construction of a man-portable oil wear analysis instrument.

  17. In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

    1996-01-01

    Remote observations of Mars have led scientists to believe that its early climate was similar to that of the early Earth, having had abundant liquid water and a dense atmosphere. One of the most fascinating questions of recent times is whether simple bacterial life developed on Mars (as it did on the Earth) during this early element period. Analyses of SNC meteorites have broadened considerably our knowledge of the chemistry of certain types of Martian rocks, underscoring the tantalizing possibility of early hydrothermal systems and even of ancient bacterial life. Detailed analyses of SNC meteorites in Terrestrial laboratories utilize the most sophisticated organic, isotopic and microscopic techniques in existence. Indeed; it is unlikely that the key biogenic indicators used in McKay et al (ibid) could be identified by a remote instrument on the surface of Mars. As a result, it is probable that any robotic search for evidence of an ancient Martian biosphere will have as its focus the identification of key minerals in likely host rocks rather than the direct detection of organic or isotopic biomarkers. Even on a sample return mission, mineralogical screening will be utilized to choose the most likely candidate rocks. X-ray diffraction (XRD) is the only technique that can provide a direct determination of the crystal structures of the phases present within a sample. When many different crystalline phases are present, quantitative analysis is better constrained if used in conjunction with a determination of elemental composition, obtainable by X-ray fluorescence (XRF) using the same X-ray source as for XRD. For planetary surface analysis, a remote instrument combining XRD and XRF could be used for mineralogical characterization of both soils and rocks. We are designing a remote XRD/XRF instrument with this objective in mind. The instrument concept pays specific attention to constraints in sample preparation, weight, volume, power, etc. Based on the geometry of a

  18. ISS Ammonia Leak Detection Through X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Camp, Jordan; Barthelmy, Scott; Skinner, Gerry

    2013-01-01

    Ammonia leaks are a significant concern for the International Space Station (ISS). The ISS has external transport lines that direct liquid ammonia to radiator panels where the ammonia is cooled and then brought back to thermal control units. These transport lines and radiator panels are subject to stress from micrometeorites and temperature variations, and have developed small leaks. The ISS can accommodate these leaks at their present rate, but if the rate increased by a factor of ten, it could potentially deplete the ammonia supply and impact the proper functioning of the ISS thermal control system, causing a serious safety risk. A proposed ISS astrophysics instrument, the Lobster X-Ray Monitor, can be used to detect and localize ISS ammonia leaks. Based on the optical design of the eye of its namesake crustacean, the Lobster detector gives simultaneously large field of view and good position resolution. The leak detection principle is that the nitrogen in the leaking ammonia will be ionized by X-rays from the Sun, and then emit its own characteristic Xray signal. The Lobster instrument, nominally facing zenith for its astrophysics observations, can be periodically pointed towards the ISS radiator panels and some sections of the transport lines to detect and localize the characteristic X-rays from the ammonia leaks. Another possibility is to use the ISS robot arm to grab the Lobster instrument and scan it across the transport lines and radiator panels. In this case the leak detection can be made more sensitive by including a focused 100-microampere electron beam to stimulate X-ray emission from the leaking nitrogen. Laboratory studies have shown that either approach can be used to locate ammonia leaks at the level of 0.1 kg/day, a threshold rate of concern for the ISS. The Lobster instrument uses two main components: (1) a microchannel plate optic (also known as a Lobster optic) that focuses the X-rays and directs them to the focal plane, and (2) a CCD (charge

  19. Screening heavy metals levels in hair of sanitation workers by X-ray fluorescence analysis.

    PubMed

    Md Khudzari, Jauharah; Wagiran, Husin; Hossain, I; Ibrahim, Noorddin

    2013-01-01

    This work presents a study of human hair as a bio-indicator for detection of heavy metals as part of environmental health surveillance programs project to develop a subject of interest in the biomedical and environmental sciences. A total of 34 hair samples were analyzed that consisting of 29 samples from sanitation workers and five samples from students. The hair samples were prepared and treated in accordance to the International Atomic Energy Agency (IAEA) recommendations. The concentrations of heavy metals were analyzed using the energy dispersive X-ray fluorescence (EDXRF) technique by X-50 Mobile X-ray Fluorescence (XRF) at Oceanography Institute, Universiti Malaysia Terengganu. The performance of EDXRF analyzer was tested by Standard Reference Material (SRM 2711) Montana Soil which was in good agreement with certified value within 14% deviations except for Hg. While seven heavy metals: Mn, Fe, Ni, Cu, Zn, Se, and Sb were detected in both groups, three additional elements, i.e. As, Hg and Pb, were detected only in sanitation workers group. For sanitation workers group, the mean concentration of six elements, Mn, Fe, Cu, Zn, Se, and Sb, shows elevated concentration as compared to the control samples concentration. Results from both groups were compared and discussed in relation to their respective heavy metals concentrations.

  20. X-ray fluorescence and absorption analysis of krypton in irradiated nuclear fuel

    NASA Astrophysics Data System (ADS)

    Degueldre, Claude; Mieszczynski, Cyprian; Borca, Camelia; Grolimund, Daniel; Martin, Matthias; Bertsch, Johannes

    2014-10-01

    The analysis of krypton in irradiated uranium dioxide fuel has been successfully achieved by X-ray fluorescence and X-ray absorption. The present study focuses on the analytical challenge of sample and sub-sample production to perform the analysis with the restricted conditions dictated by the radioprotection regulations. It deals also with all potential interferences that could affect the quality of the measurement in fluorescence as well as in absorption mode. The impacts of all dissolved gases in the fuel matrix are accounted for the analytical result quantification. The krypton atomic environment is ruled by the presence of xenon. Other gases such as residual argon and traces of helium or hydrogen are negligible. The results are given in term of density for krypton (∼3 nm-3) and xenon (∼20 nm-3). The presence of dissolved, interstitial and nano-phases are discussed together with other analytical techniques that could be applied to gain information on fission gas behaviour in nuclear fuels.

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

    NASA Astrophysics Data System (ADS)

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

    2010-02-01

    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% (1 σ) 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.

  2. Method for detecting binding events using micro-X-ray fluorescence spectrometry

    DOEpatents

    Warner, Benjamin P.; Havrilla, George J.; Mann, Grace

    2010-12-28

    Method for detecting binding events using micro-X-ray fluorescence spectrometry. Receptors are exposed to at least one potential binder and arrayed on a substrate support. Each member of the array is exposed to X-ray radiation. The magnitude of a detectable X-ray fluorescence signal for at least one element can be used to determine whether a binding event between a binder and a receptor has occurred, and can provide information related to the extent of binding between the binder and receptor.

  3. Pseudo-color enhanced x-ray fluorescence imaging of the Archimedes Palimpsest

    NASA Astrophysics Data System (ADS)

    Bergmann, Uwe; Knox, Keith T.

    2009-01-01

    A combination of x-ray fluorescence and image processing has been shown to recover text characters written in iron gall ink on parchment, even when obscured by gold paint. Several leaves of the Archimedes Palimpsest were imaged using rapid-scan, x-ray fluorescence imaging performed at the Stanford Synchrotron Radiation Lightsource of the SLAC National Accelerator Laboratory. A simple linear show-through model is shown to successfully separate different layers of text in the x-ray images, making the text easier to read by the scholars.

  4. New approach to breast tumor detection based on fluorescence x-ray analysis

    PubMed Central

    Hayashi, Yasuhiko; Okuyama, Fumio

    2010-01-01

    A new technical approach to breast-tumor detection is proposed. The technique is based on fluorescence x-ray analysis, and can identify a miniature malignant tumor within the breast. The primary beam intensity needed in fluorescence x-ray analysis is on a lower order of magnitude than that used in mammography. Thus, the newly-proposed technique would enable detection of a still tiny breast cancer while dramatically lowering the radiation dose. Field-emission x-ray sources might be a key for translating this concept into a medical technique. PMID:20930932

  5. X-ray diffraction and time-resolved fluorescence analyses of Aequorea green fluorescent protein crystals.

    PubMed

    Perozzo, M A; Ward, K B; Thompson, R B; Ward, W W

    1988-06-05

    The energy transfer protein, green fluorescent protein, from the hydromedusan jellyfish Aequorea victoria has been crystallized in two morphologies suitable for x-ray diffraction analysis. Hexagonal plates have been obtained in the P6122 or P6522 space group with a = b = 77.5, c = 370 A, and no more than three molecules per asymmetric unit. Monoclinic parallel-epipeds have been obtained in the C2 space group with a = 93.3, b = 66.5, c = 45.5 A, beta = 108 degrees, and one molecule per asymmetric unit. The monoclinic form is better suited for use in a structure determination, and a data set was collected from the native crystal. Time-resolved fluorescence measurements of large single crystals are possible due to the unique, covalently bound chromophore present in this molecule. Fluorescence emission spectra of Aequorea green fluorescent protein in solution and from either the hexagonal or monoclinic single crystal show similar profiles suggesting that the conformations of protein in solution and in the crystal are similar. Multifrequency phase fluorimetric data obtained from a single crystal were best fit by a single fluorescence lifetime very close to that exhibited by the protein in solution. The complementary structural data obtained from fluorescence spectroscopy and x-ray diffraction crystallography will aid in the elucidation of this novel protein's structure-function relationship.

  6. Contribution of inner shell Compton ionization to the X-ray fluorescence line intensity

    NASA Astrophysics Data System (ADS)

    Fernández, Jorge E.; Scot, Viviana; Di Giulio, Eugenio

    2016-10-01

    The Compton effect is a potential ionization mechanism of atoms. It produces vacancies in inner shells that are filled with the same mechanism of atomic relaxation as the one following photo-absorption. This contribution to X-ray fluorescence emission is frequently neglected because the total Compton cross-section is apparently much lower than the photoelectric one at useful X-ray energies. However, a more careful analysis suggests that is necessary to consider single shell cross sections (instead of total cross sections) as a function of energy. In this article these Compton cross sections are computed for the shells K, L1-L3 and M1-M5 in the framework of the impulse approximation. By comparing the Compton and the photoelectric cross-section for each shell it is then possible to determine the extent of the Compton correction to the intensity of the corresponding characteristic lines. It is shown that for the K shell the correction becomes relevant for excitation energies which are too high to be influent in X-ray spectrometry. In contrast, for L and M shells the Compton contribution is relevant for medium-Z elements and medium energies. To illustrate the different grades of relevance of the correction, for each ionized shell, the energies for which the Compton contribution reaches the extent levels of 1, 5, 10, 20, 50 and 100% of the photoelectric one are determined for all the elements with Z = 11-92. For practical applications it is provided a simple formula and fitting coefficients to compute average correction levels for the shells considered.

  7. Energy dispersive X-Ray fluorescence determination of thorium in phosphoric acid solutions

    NASA Astrophysics Data System (ADS)

    Mirashi, N. N.; Dhara, Sangita; Kumar, S. Sanjay; Chaudhury, Satyajeet; Misra, N. L.; Aggarwal, S. K.

    2010-07-01

    Energy dispersive X-ray fluorescence studies on determination of thorium (in the range of 7 to 137 mg/mL) in phosphoric acid solutions obtained by dissolution of thoria in autoclave were made. Fixed amounts of Y internal standard solutions, after dilution with equal amount of phosphoric acid, were added to the calibration as well as sample solutions. Solution aliquots of approximately 2-5 µL were deposited on thick absorbent sheets to absorb the solutions and the sheets were presented for energy dispersive X-ray fluorescence measurements. A calibration plot was made between intensity ratios (Th Lα/Y Kα) against respective amounts of thorium in the calibration solutions. Thorium amounts in phosphoric acid samples were determined using their energy dispersive X-ray fluorescence spectra and the above calibration plot. The energy dispersive X-ray fluorescence results, thus obtained, were compared with the corresponding gamma ray spectrometry results and were found to be within average deviation of 2.6% from the respective gamma ray spectrometry values. The average precision obtained in energy dispersive X-ray fluorescence determinations was found to be 4% (1 σ). The energy dispersive X-ray fluorescence method has an advantage over gamma ray spectrometry for thorium determination as the amount of sample required and measurement time is far less compared to that required in gamma ray spectrometry.

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

    PubMed Central

    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 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

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

    PubMed

    Ingerle, D; Meirer, F; Pepponi, G; Demenev, E; Giubertoni, D; Wobrauschek, P; Streli, C

    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

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

    NASA Astrophysics Data System (ADS)

    Ingerle, D.; Meirer, F.; Pepponi, G.; Demenev, E.; Giubertoni, D.; Wobrauschek, P.; Streli, C.

    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

  11. Tabletop Ultrabright Kiloelectronvolt X-Ray Sources from Xe and Kr Hollow Atom States

    NASA Astrophysics Data System (ADS)

    Sankar, Poopalasingam

    Albert Einstein, the father of relativity, once said, "Look deep into nature, and then you will understand everything better". Today available higher resolution tabletop tool to look deep into matters and living thing is an x-ray source. Although the available tabletop x-rays sources of the 20th century, such as the ones used for medical or dental x-rays are tremendously useful for medical diagnostics and industry, a major disadvantage is that they have low quality skillful brightness, which limits its resolution and accuracy. In the other hand, x-ray free-electrons laser (XFEL) and synchrotron radiation sources provided extreme bright x-rays. However, number of applications of XFEL and synchrotron such as medical and industrials, has been hampered by their size, complexity, and cost. This has set a goal of demonstrating x-ray source with enough brightness for potential applications in an often-called tabletop compact x-ray source that could be operated in university laboratory or hospitals. We have developed two tabletop ultrabright keV x-ray sources, one from a Xe hollow-atom states and the other one from Kr hollow-atom stares with a unique characteristic that makes them complementary to currently-available extreme-light sources; XFEL, and synchrotron x-ray source. Upgraded tabletop ultra-fast KrF* pump-laser interacts with target rare-gas clusters and produces hollow-atom states, which later coherently collapse to the empty inner-shell and thereby generate keV x-ray radiation. The KrF* pump-laser beam is self-focused and forms a self-channel to guide the generated x-ray radiation in the direction of the pump-laser beam to produce directed x-ray beam. Xe (M) x-ray source operates at 1.2-1.6 nm wavelength while the Kr(L) x-ray source operates in 600-800 pm wavelength. System is mounted upon 3 optical-tables (5´x12´) with two KrF amplifiers at a repetition rate of 0.1 Hz. A lower bound for brightness value for both Xe and Kr x-ray sources is 1026 photons s-1mm-2

  12. Optimized Detector Angular Configuration Increases the Sensitivity of X-ray Fluorescence Computed Tomography (XFCT).

    PubMed

    Ahmad, Moiz; Bazalova-Carter, Magdalena; Fahrig, Rebecca; Xing, Lei

    2015-05-01

    In this work, we demonstrated that an optimized detector angular configuration based on the anisotropic energy distribution of background scattered X-rays improves X-ray fluorescence computed tomography (XFCT) detection sensitivity. We built an XFCT imaging system composed of a bench-top fluoroscopy X-ray source, a CdTe X-ray detector, and a phantom motion stage. We imaged a 6.4-cm-diameter phantom containing different concentrations of gold solution and investigated the effect of detector angular configuration on XFCT image quality. Based on our previous theoretical study, three detector angles were considered. The X-ray fluorescence detector was first placed at 145 (°) (approximating back-scatter) to minimize scatter X-rays. XFCT image quality was compared to images acquired with the detector at 60 (°) (forward-scatter) and 90 (°) (side-scatter). The datasets for the three different detector positions were also combined to approximate an isotropically arranged detector. The sensitivity was optimized with detector in the 145 (°) back-scatter configuration counting the 78-keV gold Kβ1 X-rays. The improvement arose from the reduced energy of scattered X-ray at the 145 (°) position and the large energy separation from gold K β1 X-rays. The lowest detected concentration in this configuration was 2.5 mgAu/mL (or 0.25% Au with SNR = 4.3). This concentration could not be detected with the 60 (°) , 90 (°) , or isotropic configurations (SNRs = 1.3, 0, 2.3, respectively). XFCT imaging dose of 14 mGy was in the range of typical clinical X-ray CT imaging doses. To our knowledge, the sensitivity achieved in this experiment is the highest in any XFCT experiment using an ordinary bench-top X-ray source in a phantom larger than a mouse ( > 3 cm).

  13. X-ray emission from charge exchange of highly-charged ions in atoms and molecules

    NASA Technical Reports Server (NTRS)

    Greenwood, J. B.; Williams, I. D.; Smith, S. J.; Chutjian, A.

    2000-01-01

    Charge exchange followed by radiative stabilization are the main processes responsible for the recent observations of X-ray emission from comets in their approach to the Sun. A new apparatus was constructed to measure, in collisions of HCIs with atoms and molecules, (a) absolute cross sections for single and multiple charge exchange, and (b) normalized X-ray emission cross sections.

  14. Development and applications of an epifluorescence module for synchrotron x-ray fluorescence microprobe imaging

    SciTech Connect

    Miller, Lisa M.; Smith, Randy J.; Ruppel, Meghan E.; Ott, Cassandra H.; Lanzirotti, Antonio

    2005-06-15

    Synchrotron x-ray fluorescence (XRF) microprobe is a valuable analysis tool for imaging trace element composition in situ at a resolution of a few microns. Frequently, epifluorescence microscopy is beneficial for identifying the region of interest. To date, combining epifluorescence microscopy with x-ray microprobe has involved analyses with two different microscopes. We report the development of an epifluorescence module that is integrated into a synchrotron XRF microprobe beamline, such that visible fluorescence from a sample can be viewed while collecting x-ray microprobe images simultaneously. This unique combination has been used to identify metal accumulation in Alzheimer's disease plaques and the mineral distribution in geological samples. The flexibility of this accessory permits its use on almost any synchrotron x-ray fluorescence microprobe beamline and applications in many fields of science can benefit from this technology.

  15. Element Mapping in Organic Samples Utilizing a Benchtop X-Ray Fluorescence Emission Tomography (XFET) System

    PubMed Central

    Groll, A.; George, J.; Vargas, P.; La Rivière, P.J.; Meng, L. J.

    2015-01-01

    X-ray fluorescence computed tomography (XFCT) is an emerging imaging modality that maps the three-dimensional distribution of elements, generally metals, in ex vivo specimens and potentially in living animals and humans. Building on our previous synchrotron-based work, we experimentally explored the use of a benchtop X-ray fluorescence computed tomography system for mapping trace-metal ions in biological samples. This system utilizes a scanning pencil-beam to stimulate the object and then relies on a detection system, with single or multiple slit apertures placed in front of position-sensitive X-ray detectors, to collect the fluorescence X-rays and to form 3-D elemental map without the need for tomographic imaging reconstruction. The technique was used to generate images of the elemental distributions of a triple-tube phantom and an osmium-stained zebrafish. PMID:26705368

  16. Element Mapping in Organic Samples Utilizing a Benchtop X-Ray Fluorescence Emission Tomography (XFET) System.

    PubMed

    Groll, A; George, J; Vargas, P; La Rivière, P J; Meng, L J

    2015-10-01

    X-ray fluorescence computed tomography (XFCT) is an emerging imaging modality that maps the three-dimensional distribution of elements, generally metals, in ex vivo specimens and potentially in living animals and humans. Building on our previous synchrotron-based work, we experimentally explored the use of a benchtop X-ray fluorescence computed tomography system for mapping trace-metal ions in biological samples. This system utilizes a scanning pencil-beam to stimulate the object and then relies on a detection system, with single or multiple slit apertures placed in front of position-sensitive X-ray detectors, to collect the fluorescence X-rays and to form 3-D elemental map without the need for tomographic imaging reconstruction. The technique was used to generate images of the elemental distributions of a triple-tube phantom and an osmium-stained zebrafish.

  17. Case Studies on Facility Characterization with X-Ray Fluorescence Spectrometry

    SciTech Connect

    Kirk, K.T.; Brooksbank, R.D.; Meszaros, J.M.; Towery, W.E.

    2008-01-15

    A hand-held x-ray fluorescence (XRF) analyzer is being used to characterize facilities in support of demolition activities at the East Tennessee Technology Park (ETTP) in Oak Ridge, Tennessee. Approximately 500 facilities at the U.S. Department of Energy site are being demolished under the ETTP Decontamination and Decommissioning (D and D) project. Facility characterization is being conducted to provide data for waste profiling and identify hazards to demolition workers. XRF spectrometry is a non-destructive analytical technique used to identify and quantify the elemental composition of a substance based on the intensity of its characteristic X-ray emission wavelength or energy. The Innov-X Systems{sup R} Model XT-245S XRF analyzer used at ETTP is equipped with a silver anode x-ray tube and a Si PIN diode detector. X-rays are generated by electrical current, eliminating the need for radioactive isotopes. Electronic components can be powered by either a lithium-ion battery or an A/C adapter, and the instrument is controlled by an iPAQ{sup R} pocket personal computer. The unit has two primary operating modes. Alloy analysis mode measures percent levels of elements in metals such as a pipes, valves, equipment, or construction materials. Soil mode provides parts-per-million (ppm) quantities in bulk solids like concrete dust, residue, paint chips, or soil. The hand-held unit can analyze material in place, or it can analyze samples in a test stand by remote operation. This paper present some case studies demonstrating a variety of XRF applications for facility characterization: Metal Materials Characterization, Lead Paint Identification, Hot Spot Delineation, Bulk Solids Testing. XRF has been the analytical technique of choice for identifying metal alloy components and has also been useful in analyzing bulk materials. Limitations of XRF testing include the inability to directly analyze elements with low atomic weights. Light elements such as beryllium and aluminum do not

  18. A fluorescence XAFS measurement instrument in the soft x-ray region toward observation under operando conditions

    SciTech Connect

    Honda, M. Baba, Y.; Shimoyama, I.; Sekiguchi, T.

    2015-03-15

    X-ray absorption fine structure (XAFS) measurements are widely used for the analysis of electronic structure. Generally, XAFS in the soft X-ray region is measured under vacuum, but chemical structures under vacuum are typically different from those under operando conditions, where chemical species exhibit their function. Here, we developed an XAFS measurement instrument, as a step toward operando fluorescent, which yields XAFS measurement using synchrotron radiation in the soft X-ray region. We applied this method to analyze the local electronic structure of the sulfur atoms in L-cysteine in different pH solutions. In water at pH 7, the hydrogen atom does not dissociate from the thiol (-SH) group in L-cysteine, which forms a structure surrounded by and interacting with water molecules. The XAFS spectrum of L-cysteine in solution was altered by changing the pH. At pH 9, the hydrogen atom dissociated and a thiolate anion was formed. Although the -SH group was oxidized to SO{sub 4}{sup 2−} when L-cysteine was adsorbed on a metal surface and dried, no oxidation was observed in solution. This may be because the water molecules were densely packed and protected the -SH group from oxidation. Our results show that this instrument aimed toward operando fluorescence XAFS measurements in the soft X-ray region is useful for structural analysis of sulfur atoms in organic molecules in air and in solution. The instrument will be applied to the structural analysis of materials containing elements that have absorption edges in soft X-ray region, such as phosphorus and alkali metals (potassium and cesium). It will be also particularly useful for the analysis of samples that are difficult to handle under vacuum and materials that have specific functions in solution.

  19. Chemical Environment Effects on K[beta]/K[alpha] Intensity Ratio: An X-Ray Fluorescence Experiment on Periodic Trends

    ERIC Educational Resources Information Center

    Durham, Chaney R.; Chase, Jeffery M.; Nivens, Delana A.; Baird, William H.; Padgett, Clifford W.

    2011-01-01

    X-ray fluorescence (XRF) data from an energy-dispersive XRF instrument were used to investigate the chlorine K[alpha] and K[beta] peaks in several group 1 salts. The ratio of the peak intensity is sensitive to the local chemical environment of the chlorine atoms studied in this experiment and it shows a periodic trend for these salts. (Contains 1…

  20. Non-conventional applications of a noninvasive portable X-ray diffraction/fluorescence instrument

    NASA Astrophysics Data System (ADS)

    Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

    2016-11-01

    Noninvasive techniques have become widespread in the cultural heritage analytical domain. The popular handheld X-ray fluorescence (XRF) devices give the elemental composition of all the layers that X-rays can penetrate, but no information on how atoms are bound together or at which depth they are located. A noninvasive portable X-ray powder diffraction/X-ray fluorescence (XRD/XRF) device may offer a solution to these limitations, since it can provide information on the composition of crystalline materials. This paper introduces applications of XRD beyond simple phase recognition. The two fundamental principles for XRD are: (1) the crystallites should be randomly oriented, to ensure proper intensity to all the diffraction peaks, and (2) the material should be positioned exactly in the focal plane of the instrument, respecting its geometry, as any displacement of the sample would results in 2 θ shifts of the diffraction peaks. In conventional XRD, the sample is ground and set on the properly positioned sample holder. Using a noninvasive portable instrument, these two requirements are seldom fulfilled. The position, size and orientation of a given crystallite within a layered structure depend on the object itself. Equation correlating the displacement (distance from the focal plane) versus peak shift (angular difference in 2 θ from the standard value) is derived and used to determine the depth at which a given substance is located. The quantitative composition of two binary Cu/Zn alloys, simultaneously present, was determined measuring the cell volume and using Vegard's law. The analysis of the whole object gives information on the texture and possible preferred orientations of the crystallites, which influences the peak intensity. This allows for the distinction between clad and electroplated daguerreotypes in the case of silver and between ancient and modern gilding for gold. Analyses of cross sections can be carried out successfully. Finally, beeswax, used in

  1. Inorganic chemical investigation by x-ray fluorescence analysis: The Viking Mars Lander

    USGS Publications Warehouse

    Toulmin, P.; Baird, A.K.; Clark, B. C.; Keil, Klaus; Rose, H.J.

    1973-01-01

    The inorganic chemical investigation added in August 1972 to the Viking Lander scientific package will utilize an energy-dispersive X-ray fluorescence spectrometer in which four sealed, gas-filled proportional counters will detect X-rays emitted from samples of the Martian surface materials irradiated by X-rays from radioisotope sources (55Fe and 109Cd). The output of the proportional counters will be subjected to pulse-height analysis by an on-board step-scanning single-channel analyzer with adjustable counting periods. The data will be returned to Earth, via the Viking Orbiter relay system, and the spectra constructed, calibrated, and interpreted here. The instrument is inside the Lander body, and samples are to be delivered to it by the Viking Lander Surface Sampler. Calibration standards are an integral part of the instrument. The results of the investigation will characterize the surface materials of Mars as to elemental composition with accuracies ranging from a few tens of parts per million (at the trace-element level) to a few percent (for major elements) depending on the element in question. Elements of atomic number 11 or less are determined only as a group, though useful estimates of their individual abundances maybe achieved by indirect means. The expected radiation environment will not seriously hamper the measurements. Based on the results, inferences can be drawn regarding (1) the surface mineralogy and lithology; (2) the nature of weathering processes, past and present, and the question of equilibrium between the atmosphere and the surface; and (3) the extent and type of differentiation that the planet has undergone. The Inorganic Chemical Investigation supports and is supported by most other Viking Science investigations. ?? 1973.

  2. Bridging the micro-to-macro gap: a new application for micro X-ray fluorescence.

    PubMed

    Davis, Jeffrey M; Newbury, Dale E; Fahey, Albert; Ritchie, Nicholas W M; Vicenzi, Edward; Bentz, Dale

    2011-06-01

    X-ray elemental mapping and X-ray spectrum imaging are powerful microanalytical tools. However, their scope is often limited spatially by the raster area of a scanning electron microscope or microprobe. Limited sampling size becomes a significant issue when large area (>10 cm²), heterogeneous materials such as concrete samples or others must be examined. In such specimens, macro-scale structures, inclusions, and concentration gradients are often of interest, yet microbeam methods are insufficient or at least inefficient for analyzing them. Such requirements largely exclude the samples of interest presented in this article from electron probe microanalysis. Micro X-ray fluorescence-X-ray spectrum imaging (μXRF-XSI) provides a solution to the problem of macro-scale X-ray imaging through an X-ray excitation source, which can be used to analyze a variety of large specimens without many of the limitations found in electron-excitation sources. Using a mid-sized beam coupled with an X-ray excitation source has a number of advantages, such as the ability to work at atmospheric pressure and lower limits of detection owing to the absence of electron-induced bremsstrahlung. μXRF-XSI also acts as a complement, where applicable, to electron microbeam X-ray output, highlighting areas of interest for follow-up microanalysis at a finer length scale.

  3. X-ray Fluorescence Spectroscopy: the Potential of Astrophysics-developed Techniques

    NASA Astrophysics Data System (ADS)

    Elvis, M.; Allen, B.; Hong, J.; Grindlay, J.; Kraft, R.; Binzel, R. P.; Masterton, R.

    2012-12-01

    X-ray fluorescence from the surface of airless bodies has been studied since the Apollo X-ray fluorescence experiment mapped parts of the lunar surface in 1971-1972. That experiment used a collimated proportional counter with a resolving power of ~1 and a beam size of ~1degree. Filters separated only Mg, Al and SI lines. We review progress in X-ray detectors and imaging for astrophysics and show how these advances enable much more powerful use of X-ray fluorescence for the study of airless bodies. Astrophysics X-ray instrumentation has developed enormously since 1972. Low noise, high quantum efficiency, X-ray CCDs have flown on ASCA, XMM-Newton, the Chandra X-ray Observatory, Swift and Suzaku, and are the workhorses of X-ray astronomy. They normally span 0.5 to ~8 keV with an energy resolution of ~100 eV. New developments in silicon based detectors, especially individual pixel addressable devices, such as CMOS detectors, can withstand many orders of magnitude more radiation than conventional CCDs before degradation. The capability of high read rates provides dynamic range and temporal resolution. Additionally, the rapid read rates minimize shot noise from thermal dark current and optical light. CMOS detectors can therefore run at warmer temperatures and with ultra-thin optical blocking filters. Thin OBFs mean near unity quantum efficiency below 1 keV, thus maximizing response at the C and O lines.such as CMOS detectors, promise advances. X-ray imaging has advanced similarly far. Two types of imager are now available: specular reflection and coded apertures. X-ray mirrors have been flown on the Einstein Observatory, XMM-Newton, Chandra and others. However, as X-ray reflection only occurs at small (~1degree) incidence angles, which then requires long focal lengths (meters), mirrors are not usually practical for planetary missions. Moreover the field of view of X-ray mirrors is comparable to the incident angle, so can only image relatively small regions. More useful

  4. Americium characterization by X-ray fluorescence and absorption spectroscopy in plutonium uranium mixed oxide

    NASA Astrophysics Data System (ADS)

    Degueldre, Claude; Cozzo, Cedric; Martin, Matthias; Grolimund, Daniel; Mieszczynski, Cyprian

    2013-06-01

    Plutonium uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The actinides in these fuels need to be analyzed after irradiation for assessing their behaviour with regard to their environment and the coolant. In this work the study of the atomic structure and next-neighbour environment of Am in the (Pu,U)O2 lattice in an irradiated (60 MW d kg-1) MOX sample was performed employing micro-X-ray fluorescence (µ-XRF) and micro-X-ray absorption fine structure (µ-XAFS) spectroscopy. The chemical bonds, valences and stoichiometry of Am (˜0.66 wt%) are determined from the experimental data gained for the irradiated fuel material examined in its peripheral zone (rim) of the fuel. In the irradiated sample Am builds up as Am3+ species within an [AmO8]13- coordination environment (e.g. >90%) and no (<10%) Am(IV) or (V) can be detected in the rim zone. The occurrence of americium dioxide is avoided by the redox buffering activity of the uranium dioxide matrix.

  5. Combined X-ray Microfluorescence and Atomic Force Microscopy Studies of Mg Distribution in Whole Cells

    SciTech Connect

    Lagomarsino, S.; Farruggia, G.; Trapani, V.; Mastrototaro, L.; Wolf, F.; Cedola, A.; Fratini, M.; Notargiacomo, A.; Bukreeva, I.; McNulty, I.; Vogt, S.; Kim, S.; Legnini, D.; Maier, J. A. M.

    2011-09-09

    We present in this paper a novel methodology that combines scanning x-ray fluorescencee microscopy and atomic force microscopy. The combination of these two techniques allows the determination of a concentration map of Mg in whole (not sectioned) cells.

  6. Monte Carlo simulation applied in total reflection x-ray fluorescence: Preliminary results

    SciTech Connect

    Meira, Luiza L. C.; Inocente, Guilherme F.; Vieira, Leticia D.; Mesa, Joel

    2013-05-06

    The X-ray Fluorescence (XRF) analysis is a technique for the qualitative and quantitative determination of chemical constituents in a sample. This method is based on detection of the characteristic radiation intensities emitted by the elements of the sample, when properly excited. A variant of this technique is the Total Reflection X-ray Fluorescence (TXRF) that utilizes electromagnetic radiation as excitation source. In total reflection of X-ray, the angle of refraction of the incident beam tends to zero and the refracted beam is tangent to the sample support interface. Thus, there is a minimum angle of incidence at which no refracted beam exists and all incident radiation undergoes total reflection. In this study, we evaluated the influence of the energy variation of the beam of incident x-rays, using the MCNPX code (Monte Carlo NParticle) based on Monte Carlo method.

  7. Versatile atomic force microscopy setup combined with micro-focused X-ray beam

    NASA Astrophysics Data System (ADS)

    Slobodskyy, T.; Zozulya, A. V.; Tholapi, R.; Liefeith, L.; Fester, M.; Sprung, M.; Hansen, W.

    2015-06-01

    Micro-focused X-ray beams produced by third generation synchrotron sources offer new perspective of studying strains and processes at nanoscale. Atomic force microscope setup combined with a micro-focused synchrotron beam allows precise positioning and nanomanipulation of nanostructures under illumination. In this paper, we report on integration of a portable commercial atomic force microscope setup into a hard X-ray synchrotron beamline. Details of design, sample alignment procedure, and performance of the setup are presented.

  8. Versatile atomic force microscopy setup combined with micro-focused X-ray beam

    SciTech Connect

    Slobodskyy, T. Tholapi, R.; Liefeith, L.; Hansen, W.; Zozulya, A. V. Fester, M.; Sprung, M.

    2015-06-15

    Micro-focused X-ray beams produced by third generation synchrotron sources offer new perspective of studying strains and processes at nanoscale. Atomic force microscope setup combined with a micro-focused synchrotron beam allows precise positioning and nanomanipulation of nanostructures under illumination. In this paper, we report on integration of a portable commercial atomic force microscope setup into a hard X-ray synchrotron beamline. Details of design, sample alignment procedure, and performance of the setup are presented.

  9. Apollo 16 geochemical X-ray fluorescence experiment: Preliminary report

    NASA Technical Reports Server (NTRS)

    Adler, I.; Trombka, J.; Gerard, J.; Lowman, P.; Schmadebeck, R.; Blodgett, H.; Eller, E.; Yin, L.; Lamothe, R.; Osswald, G.

    1972-01-01

    The lunar surface was mapped with respect to Mg, Al, and Si, as Al/Si and Mg/Si ratios along the projected ground tracks swept out by the orbiting Apollo 16 spacecraft. The results confirm the observations made during the Apollo 15 flight and provide data for a number of features not covered before. The data are consistent with the idea that the moon has a widespread differentiated crust (the highlands). The Al/Si and Mg/Si chemical ratios correspond to that for anorthositic gabbro through gabbroic anorthosites or feldspathic basalts. The X-ray results suggest the occurrence of this premare crust or material similar to it as the Descartes landing site.

  10. Apollo 16 Geochemical X-ray Fluorescence Experiment: Preliminary Report.

    PubMed

    Adler, I; Trombka, J; Gerard, J; Lowman, P; Schmadebeck, R; Blodget, H; Eller, E; Yin, L; Lamothe, R; Osswald, G; Gorenstein, P; Bjorkholm, P; Gursky, H; Harris, B

    1972-07-21

    The lunar surface was mapped with respect to magnesium, aluminum, and silicon as aluminum/ silicon and magnesium/ silicon intensity ratios along the projected ground tracks swept out by the orbiting Apollo 16 spacecraft. The results confirm the observations made during the Apollo 15 flight and provide new data for a number of features not covered before. The data are consistent with the idea that the moon has a widespread differentiated crust (the highlands). The aluminum/ silicon and magnesium/ silicon concentration ratios correspond to those for anorthositic gabbros through gabbroic anorthosites or feldspathic basalts. The x-ray results suggest the occurrence of this premare crust or material similar to it at the Descartes landing site.

  11. Geometrical factor correction in grazing incident x-ray fluorescence experiment

    SciTech Connect

    Li Wenbin; Zhu Jingtao; Ma Xiaoying; Li Haochuan; Wang Hongchang; Wang Zhanshan; Sawhney, Kawal J. S.

    2012-05-15

    The geometrical factor in the grazing incident x-ray fluorescence analysis is an important angle-dependent term, which can have a great effect on the measured data. In this paper, the effects of the geometrical factor on the florescence yield have been demonstrated. A formula is presented to estimate the geometrical factor, which includes the experimental parameters of the beam and setup. The validity of this formula is proven by the good agreement between the calculated fluorescence yields with the experimental results in grazing incident x-ray fluorescence analysis.

  12. Portable x-ray fluorescence spectrometer for environmental monitoring of inorganic pollutants

    NASA Technical Reports Server (NTRS)

    Thornton, Michael G. (Inventor); Clark, III, Benton C. (Inventor)

    1991-01-01

    A portable x-ray fluorescence spectrometer has a portable sensor unit containing a battery, a high voltage power supply, an x-ray tube which produces a beam x-ray radiation directed toward a target sample, and a detector for fluorescent x-rays produced by the sample. If a silicon-lithium detector is used, the sensor unit also contains either a thermoelectric or thermochemical cooler, or a small dewar flask containing liquid nitrogen to cool the detector. A pulse height analyzer (PHA) generates a spectrum of data for each sample consisting of the number of fluorescent x-rays detected as a function of their energy level. The PHA can also store spectrum data for a number of samples in the field. A processing unit can be attached to the pulse height analyzer to upload and analyze the stored spectrum data for each sample. The processing unit provides a graphic display of the spectrum data for each sample, and provides qualitative and/or quantitative analysis of the elemental composition of the sample by comparing the peaks in the sample spectrum against known x-ray energies for various chemical elements. An optional filtration enclosure can be used to filter particles from a sample suspension, either in the form of a natural suspension or a chemically created precipitate. The sensor unit is then temporarily attached to the filtration unit to analyze the particles collected by the filter medium.

  13. Design and characterization of a pulsed x ray source for fluorescent lifetime measurements

    NASA Astrophysics Data System (ADS)

    Blankespoor, S. C.

    1993-12-01

    To search for new, fast, inorganic scintillators, the author and his colleagues have developed a bench-top pulsed x-ray source for determining fluorescent lifetimes and wavelengths of compounds in crystal or powdered form. This source uses a light-excited x-ray tube which produces x-rays when light from a laser diode strikes its photocathode. The x-ray tube has a tungsten anode, a beryllium exit window, a 30 kV maximum tube bias, and a 50 HA maximum average cathode current. The laser produces 3 x 10(exp 7) photons at 650 nm per approximately 100 ps pulse, with up to 10(exp 7) pulses/sec. The time spread for the laser diode, x-ray tube, and a microchannel plate photomultiplier tube is less than 120 ps fwhm. The mean x-ray photon energy, at tube biases of 20, 25, and 30 kV, is 9.4, 10.3, and 11.1 keV, respectively. They measured 140, 230, and 330 x-ray photons per laser diode pulse per steradian at tube biases of 20, 25, and 30 kV, respectively. Background x-rays due to dark current occur at a rate of 1 x 10(exp 6) and 3 x 10(exp 6) photons/sec/steradian at tube biases of 25 and 30 kV, respectively. Data characterizing the x-ray output with an aluminum filter in the x-ray beam are also presented.

  14. Design and characterization of a pulsed x-ray source for fluorescent lifetime measurements

    SciTech Connect

    Blankespoor, S.C. |

    1993-12-01

    To search for new, fast, inorganic scintillators, the author and his colleagues have developed a bench-top pulsed x-ray source for determining fluorescent lifetimes and wavelengths of compounds in crystal or powdered form. This source uses a light-excited x-ray tube which produces x-rays when light from a laser diode strikes its photocathode. The x-ray tube has a tungsten anode, a beryllium exit window, a 30 kV maximum tube bias, and a 50 HA maximum average cathode current. The laser produces 3 {times} 10{sup 7} photons at 650 nm per {approximately}100 ps pulse, with up to 10{sup 7} pulses/sec. The time spread for the laser diode, x-ray tube, and a microchannel plate photomultiplier tube is less than 120 ps fwhm. The mean x-ray photon energy, at tube biases of 20, 25, and 30 kV, is 9.4, 10.3, and 11.1 keV, respectively. They measured 140, 230, and 330 x-ray photons per laser diode pulse per steradian at tube biases of 20, 25, and 30 kV, respectively. Background x-rays due to dark current occur at a rate of 1 {times} 10{sup 6} and 3 {times} 10{sup 6} photons/sec/steradian at tube biases of 25 and 30 kV, respectively. Data characterizing the x-ray output with an aluminum filter in the x-ray beam are also presented.

  15. Simultaneous x-ray fluorescence and K-edge CT imaging with photon-counting detectors

    NASA Astrophysics Data System (ADS)

    Li, Liang; Li, Ruizhe; Zhang, Siyuan; Chen, Zhiqiang

    2016-10-01

    Rapid development of the X-ray phonon-counting detection technology brings tremendous research and application opportunities. In addition to improvements in conventional X-ray imaging performance such as radiation dose utilization and beam hardening correction, photon-counting detectors allows significantly more efficient X-ray fluorescence (XRF) and K-edge imaging, and promises a great potential of X-ray functional, cellular and molecular imaging. XRF is the characteristic emission of secondary X-ray photons from a material excited by initial X-rays. The phenomenon is widely used for chemical and elemental analysis. K-edge imaging identifies a material based on its chemically-specific absorption discontinuity over X-ray photon energy. In this paper, we try to combine XRF and K-edge signals from the contrast agents (e.g., iodine, gadolinium, gold nanoparticles) to simultaneously realize XFCT and K-edge CT imaging for superior image performance. As a prerequisite for this dual-modality imaging, the accurate energy calibration of multi-energy-bin photon-counting detectors is critically important. With the measured XRF data of different materials, we characterize the energy response function of a CZT detector for energy calibration and spectrum reconstruction, which can effectively improve the energy resolution and decrease the inconsistence of the photon counting detectors. Then, a simultaneous K-edge and X-ray fluorescence CT imaging (SKYFI) experimental setup is designed which includes a cone-beam X-ray tube, two separate photon counting detector arrays, a pin-hole collimator and a rotation stage. With a phantom containing gold nanoparticles the two types of XFCT and K-edge CT datasets are collected simultaneously. Then, XFCT and K-edge CT images are synergistically reconstructed in a same framework. Simulation results are presented and quantitative analyzed and compared with the separate XFCT and K-edge CT results.

  16. Determination of trace elements in Syrian medicinal plants and their infusions by energy dispersive X-ray fluorescence and total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Khuder, A.; Sawan, M. Kh.; Karjou, J.; Razouk, A. K.

    2009-07-01

    X-ray fluorescence (XRF) and total-reflection X-ray fluorescence (TXRF) techniques suited well for a multi-element determination of K, Ca, Mn, Fe, Cu, Zn, Rb, and Sr in some Syrian medicinal plant species. The accuracy and the precision of both techniques were verified by analyzing the Standard Reference Materials (SRM) peach-1547 and apple leaves-1515. A good agreement between the measured concentrations of the previously mentioned elements and the certified values were obtained with errors less than 10.7% for TXRF and 15.8% for XRF. The determination of Br was acceptable only by XRF with an error less than 24%. Furthermore, the XRF method showed a very good applicability for the determination of K, Ca, Mn, Fe, Cu, Zn, Rb, Sr, and Br in infusions of different Syrian medicinal plant species, namely anise ( Anisum vulgare), licorice root ( Glycyrrhiza glabra), and white wormwood ( Artemisia herba-alba).

  17. X-ray fluorescence and energy dispersive x-ray diffraction for the quantification of elemental concentrations in breast tissue.

    PubMed

    Geraki, K; Farquharson, M J; Bradley, D A

    2004-01-07

    This paper presents improvements on a previously reported method for the measurement of elements in breast tissue specimens (Geraki et al 2002 Phys. Med. Biol. 47 2327-39). A synchrotron-based system was used for the detection of the x-ray fluorescence (XRF) emitted from iron, copper, zinc and potassium in breast tissue specimens, healthy and cancerous. Calibration models resulting from the irradiation of standard aqueous solutions were used for the quantification of the elements. The present developments concentrate on increasing the convergence between the tissue samples and the calibration models, therefore improving accuracy. For this purpose the composition of the samples in terms of adipose and fibrous tissue was evaluated, using an energy dispersive x-ray diffraction (EDXRD) system. The relationships between the attenuation and scatter properties of the two tissue components and water were determined through Monte Carlo simulations. The results from the simulations and the EDXRD measurements allowed the XRF data from each specimen to be corrected according to its composition. The statistical analysis of the elemental concentrations of the different groups of specimens reveals that all four elements are found in elevated levels in the tumour specimens. The increase is less pronounced for iron and copper and most for potassium and zinc. Other observed features include the substantial degree of inhomogeneity of elemental distributions within the volume of the specimens, varying between 4% and 36% of the mean, depending on the element and the type of the sample. The accuracy of the technique, based on the measurement of a standard reference material, proved to be between 3% and 22% depending on the element, which presents only a marginal improvement (1%-3%) compared to the accuracy of the previously reported results. The measurement precision was between 1% and 9% while the calculated uncertainties on the final elemental concentrations ranged between 10% and 16%.

  18. Determination of copper nanoparticle size distributions with total reflection X-ray fluorescence spectroscopy.

    PubMed

    Singh, Andy; Luening, Katharina; Brennan, Sean; Homma, Takayuki; Kubo, Nobuhiro; Nowak, Stanisław H; Pianetta, Piero

    2017-01-01

    Total reflection X-ray fluorescence (TXRF) analysis is extensively used by the semiconductor industry for measuring trace metal contamination on silicon surfaces. In addition to determining the quantity of impurities on a surface, TXRF can reveal information about the vertical distribution of contaminants by measuring the fluorescence signal as a function of the angle of incidence. In this study, two samples were intentionally contaminated with copper in non-deoxygenated and deoxygenated ultrapure water (UPW) resulting in impurity profiles that were either atomically dispersed in a thin film or particle-like, respectively. The concentration profile of the samples immersed into deoxygenated UPW was calculated using a theoretical concentration profile representative of particles, yielding a mean particle height of 16.1 nm. However, the resulting theoretical profile suggested that a distribution of particle heights exists on the surface. The fit of the angular distribution data was further refined by minimizing the residual error of a least-squares fit employing a model with a Gaussian distribution of particle heights about the mean height. The presence of a height distribution was also confirmed with atomic force microscopy measurements.

  19. New Directions in X-Ray Light Sources or Fiat Lux: what's under the dome and watching atoms with x-rays (LBNL Summer Lecture Series)

    SciTech Connect

    Falcone, Roger

    2008-07-15

    Summer Lecture Series 2008: Molecular movies of chemical reactions and material phase transformations need a strobe of x-rays, the penetrating light that reveals how atoms and molecules assemble in chemical and biological systems and complex materials. Roger Falcone, Director of the Advanced Light Source,will discuss a new generation of x ray sources that will enable a new science of atomic dynamics on ultrafast timescales.

  20. New Directions in X-Ray Light Sources or Fiat Lux: what's under the dome and watching atoms with x-rays (LBNL Summer Lecture Series)

    ScienceCinema

    Falcone, Roger

    2016-07-12

    Summer Lecture Series 2008: Molecular movies of chemical reactions and material phase transformations need a strobe of x-rays, the penetrating light that reveals how atoms and molecules assemble in chemical and biological systems and complex materials. Roger Falcone, Director of the Advanced Light Source,will discuss a new generation of x ray sources that will enable a new science of atomic dynamics on ultrafast timescales.

  1. X-Ray Elastic and Inelastic Scattering Factors for Neutral Atoms Z = 2-92

    NASA Astrophysics Data System (ADS)

    Wang, J. H.; Sagar, R. P.; Schmider, H.; Smith, V. H.

    1993-03-01

    X-ray elastic and inelastic scattering factors are calculated for the ground states of the neutral atoms, helium to uranium, from the Roothaan-Hartree-Fock nonrelativistic self-consistent-field wave functions of Clementi and Roetti, (Atomic Data and Nuclear Data Tables 14, 177, 1974) and McLean and McLean (Atomic Data and Nuclear Data Tables 26, 197, 1981).

  2. TU-G-207-03: High Spatial Resolution and High Sensitivity X-Ray Fluorescence Imaging

    SciTech Connect

    Xing, L.

    2015-06-15

    Last few years has witnessed the development of novel of X-ray imaging modalities, such as spectral CT, phase contrast CT, and X-ray acoustic/fluorescence/luminescence imaging. This symposium will present the recent advances of these emerging X-ray imaging modalities and update the attendees with knowledge in various related topics, including X-ray photon-counting detectors, X-ray physics underlying the emerging applications beyond the traditional X-ray imaging, image reconstruction for the novel modalities, characterization and evaluation of the systems, and their practical implications. In addition, the concept and practical aspects of X-ray activatable targeted nanoparticles for molecular X-ray imaging will be discussed in the context of X-ray fluorescence and luminescence CT. Learning Objectives: Present background knowledge of various emerging X-ray imaging techniques, such as spectral CT, phase contrast CT and X-ray fluorescence/luminescence CT. Discuss the practical need, technical aspects and current status of the emerging X-ray imaging modalities. Describe utility and future impact of the new generation of X-ray imaging applications.

  3. Quantitative measurement of binary liquid distributions using multiple-tracer x-ray fluorescence and radiography

    SciTech Connect

    Halls, Benjamin R.; Meyer, Terrence R.; Kastengren, Alan L.

    2015-01-01

    The complex geometry and large index-of-refraction gradients that occur near the point of impingement of binary liquid jets present a challenging environment for optical interrogation. A simultaneous quadruple-tracer x-ray fluorescence and line-of-sight radiography technique is proposed as a means of distinguishing and quantifying individual liquid component distributions prior to, during, and after jet impact. Two different pairs of fluorescence tracers are seeded into each liquid stream to maximize their attenuation ratio for reabsorption correction and differentiation of the two fluids during mixing. This approach for instantaneous correction of x-ray fluorescence reabsorption is compared with a more time-intensive approach of using stereographic reconstruction of x-ray attenuation along multiple lines of sight. The proposed methodology addresses the need for a quantitative measurement technique capable of interrogating optically complex, near-field liquid distributions in many mixing systems of practical interest involving two or more liquid streams.

  4. Analysis of eight argonne premium coal samples by X-ray fluorescence spectrometry

    USGS Publications Warehouse

    Evans, J.R.; Sellers, G.A.; Johnson, R.G.; Vivit, D.V.; Kent, J.

    1990-01-01

    X-ray fluorescence spectrometric methods were used in the analysis of eight Argonne Premium Coal Samples. Trace elements (Cr, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Ba, La, and Ce) in coal ash were determined by energy-dispersive X-ray fluorescence spectrometry; major elements (Na, Mg, Al, Si, P, S, K, Ca, Ti, Mn, and Fe) in coal ash and trace elements (Cl and P) in whole coal were determined by wavelength-dispersive X-ray fluorescence spectrometry. The results of this study will be used in a geochemical database compiled for these materials from various analytical techniques. The experimental XRF methods and procedures used to determine these major and trace elements are described.

  5. Demonstration of x-ray fluorescence imaging of a high-energy-density plasma

    SciTech Connect

    MacDonald, M. J. Gamboa, E. J.; Keiter, P. A.; Fein, J. R.; Klein, S. R.; Kuranz, C. C.; LeFevre, H. J.; Manuel, M. J.-E.; Wan, W. C.; Drake, R. P.; Montgomery, D. S.; Biener, M. M.; Fournier, K. B.; Streit, J.

    2014-11-15

    Experiments at the Trident Laser Facility have successfully demonstrated the use of x-ray fluorescence imaging (XRFI) to diagnose shocked carbonized resorcinol formaldehyde (CRF) foams doped with Ti. One laser beam created a shock wave in the doped foam. A second laser beam produced a flux of vanadium He-α x-rays, which in turn induced Ti K-shell fluorescence within the foam. Spectrally resolved 1D imaging of the x-ray fluorescence provided shock location and compression measurements. Additionally, experiments using a collimator demonstrated that one can probe specific regions within a target. These results show that XRFI is a capable alternative to path-integrated measurements for diagnosing hydrodynamic experiments at high energy density.

  6. Elemental mapping in a contemporary miniature by full-field X-ray fluorescence imaging with gaseous detector vs. scanning X-ray fluorescence imaging with polycapillary optics

    NASA Astrophysics Data System (ADS)

    Silva, A. L. M.; Cirino, S.; Carvalho, M. L.; Manso, M.; Pessanha, S.; Azevedo, C. D. R.; Carramate, L. F. N. D.; Santos, J. P.; Guerra, M.; Veloso, J. F. C. A.

    2017-03-01

    Energy dispersive X-ray imaging can be used in several research fields and industrial applications. Elemental mapping through energy dispersive X-ray imaging technique has become a promising method to obtain positional distribution of specific elements in a non-destructive way. To obtain the elemental distribution of a sample it is necessary to use instruments capable of providing a precise positioning together with a good energy resolution. Polycapillary beams together with silicon drift chamber detectors are used in several commercial systems and are considered state-of-the-art spectrometers, however they are usually very costly. A new concept of large energy dispersive X-ray imaging systems based on gaseous radiation detectors emerged in the last years enabling a promising 2D elemental detection at a very reduced price. The main goal of this work is to analyze a contemporary Indian miniature with both X-ray fluorescence imaging systems, the one based on a gaseous detector 2D-THCOBRA and the state-of-the-art spectrometer M4 Tornado, from Bruker. The performance of both systems is compared and evaluated in the context of the sample's analysis.

  7. Spectrally resolving and scattering-compensated x-ray luminescence/fluorescence computed tomography

    PubMed Central

    Cong, Wenxiang; Shen, Haiou; Wang, Ge

    2011-01-01

    The nanophosphors, or other similar materials, emit near-infrared (NIR) light upon x-ray excitation. They were designed as optical probes for in vivo visualization and analysis of molecular and cellular targets, pathways, and responses. Based on the previous work on x-ray fluorescence computed tomography (XFCT) and x-ray luminescence computed tomography (XLCT), here we propose a spectrally-resolving and scattering-compensated x-ray luminescence/fluorescence computed tomography (SXLCT or SXFCT) approach to quantify a spatial distribution of nanophosphors (other similar materials or chemical elements) within a biological object. In this paper, the x-ray scattering is taken into account in the reconstruction algorithm. The NIR scattering is described in the diffusion approximation model. Then, x-ray excitations are applied with different spectra, and NIR signals are measured in a spectrally resolving fashion. Finally, a linear relationship is established between the nanophosphor distribution and measured NIR data using the finite element method and inverted using the compressive sensing technique. The numerical simulation results demonstrate the feasibility and merits of the proposed approach. PMID:21721815

  8. A high-resolution large-acceptance analyzer for X-ray fluorescence and Raman spectroscopy

    SciTech Connect

    Bergmann, Uwe; Cramer, Stephen P.

    2001-08-02

    A newly designed multi-crystal X-ray spectrometer and its applications in the fields of X-ray fluorescence and X-ray Raman spectroscopy are described. The instrument is based on 8 spherically curved Si crystals, each with a 3.5 inch diameter form bent to a radius of 86 cm. The crystals are individually aligned in the Rowland geometry capturing a total solid angle of 0.07 sr. The array is arranged in a way that energy scans can be performed by moving the whole instrument, rather than scanning each crystal by itself. At angles close to back scattering the energy resolution is between 0.3 and 1 eV depending on the beam dimensions at the sample. The instrument is mainly designed for X-ray absorption and fluorescence spectroscopy of transition metals in dilute systems such as metalloproteins. First results of the Mn K{beta} (3p -> 1s) emission in photosystem II are shown. An independent application of the instrument is the technique of X-ray Raman spectroscopy which can address problems similar to those in traditional soft X-ray absorption spectroscopies, and initial results are presented.

  9. Imaging Nonequilibrium Atomic Vibrations with X-ray Diffuse Scattering

    SciTech Connect

    Trigo, M.; Chen, J.; Vishwanath, V.H.; Sheu, Y.M.; Graber, T.; Henning, R.; Reis, D; /SLAC /Stanford U., Appl. Phys. Dept.

    2011-03-03

    We use picosecond x-ray diffuse scattering to image the nonequilibrium vibrations of the lattice following ultrafast laser excitation. We present images of nonequilibrium phonons in InP and InSb throughout the Brillouin-zone which remain out of equilibrium up to nanoseconds. The results are analyzed using a Born model that helps identify the phonon branches contributing to the observed features in the time-resolved diffuse scattering. In InP this analysis shows a delayed increase in the transverse acoustic (TA) phonon population along high-symmetry directions accompanied by a decrease in the longitudinal acoustic (LA) phonons. In InSb the increase in TA phonon population is less directional.

  10. Refraction and absorption of x rays by laser-dressed atoms.

    SciTech Connect

    Buth, C.; Santra, R.; Young, L.

    2010-06-01

    X-ray refraction and absorption by neon atoms under the influence of an 800 nm laser with an intensity of 10{sup 13} W/cm{sup 2} is investigated. For this purpose, we use an ab initio theory suitable for optical strong-field problems. Its results are interpreted in terms of a three-level model. On the Ne 1s {yields} 3p resonance, we find electromagnetically induced transparency (EIT) for x rays. Our work opens novel perspectives for ultrafast x-ray pulse shaping.

  11. X-RAY FLUORESCENCE ANALYSIS OF HANFORD LOW ACTIVITY WASTE SIMULANTS METHOD DEVELOPMENT

    SciTech Connect

    Jurgensen, A; David Missimer, D; Ronny Rutherford, R

    2007-08-08

    The x-ray fluorescence laboratory (XRF) in the Analytical Development Directorate (ADD) of the Savannah River National Laboratory (SRNL) was requested to develop an x-ray fluorescence spectrometry method for elemental characterization of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) pretreated low activity waste (LAW) stream to the LAW Vitrification Plant. The WTP is evaluating the potential for using XRF as a rapid turnaround technique to support LAW product compliance and glass former batching. The overall objective of this task was to develop an XRF analytical method that provides rapid turnaround time (<8 hours), while providing sufficient accuracy and precision to determine variations in waste.

  12. Dense Heavy Metal Aerosol Monitoring by Direct X-Ray Fluorescence

    DTIC Science & Technology

    1989-06-01

    TECHNICAL REPORT BRL-TR-3003 BRL 0 sDENSE HEAVY METAL AEROSOL MONITORING BY DIRECT X-RAY FLUORESCENCE I GEORGE M. THOMSON flgDTIC ELF% CTE b JUN 16...21005-5066 /F 6261A jIN8 1001I 11. TITLE (-’mi- Sawt Cauif&aan)II DENSE HEAVY METAL AEROSOL MONITORMN BY DIRECT X-RAY FLUORESCENCE 12. PERSONAL AUTHOR(S...Before proceeding, a definition of the term "dense, heavy - metal aerosol" is in order. For present purposes, it is an aerosol in which the suspended

  13. Application of X-ray fluorescence in an investigation of photographic heritage

    NASA Astrophysics Data System (ADS)

    Čechák, T.; Kopecká, I.; Trojek, T.; Štanzel, T.; Bártová, H.

    2015-11-01

    X-ray fluorescence analysis uses ionizing radiation to study the elemental composition of materials. It is widely used for many purposes, including studies of various cultural and historic relicts and objects of art. This paper summarizes our experience with X-ray fluorescence analysis and attenuated total reflectance Fourier transform infrared spectroscopy in investigating historical photographs by means of portable spectroscopic devices. The results of these measurements provide information about the composition of historical photographs and their toning. They can be used for comparing the processes used in fabricating the photographs, for assessing the quality of the paper and, in many cases, for information about how to repair damaged parts.

  14. Improving accuracy and capabilities of X-ray fluorescence method using intensity ratios

    NASA Astrophysics Data System (ADS)

    Garmay, Andrey V.; Oskolok, Kirill V.

    2017-04-01

    An X-ray fluorescence analysis algorithm is proposed which is based on a use of ratios of X-ray fluorescence lines intensities. Such an analytical signal is more stable and leads to improved accuracy. Novel calibration equations are proposed which are suitable for analysis in a broad range of matrix compositions. To apply the algorithm to analysis of samples containing significant amount of undetectable elements a use of a dependence of a Rayleigh-to-Compton intensity ratio on a total content of these elements is suggested. The technique's validity is shown by analysis of standard steel samples, model metal oxides mixture and iron ore samples.

  15. First X-ray Fluorescence MicroCT Results from Micrometeorites at SSRL

    SciTech Connect

    Ignatyev, K; Huwig, K; Harvey, R; Ishii, H; Bradley, J; Luening, K; Brennan, S; Pianetta, P

    2006-08-23

    X-ray fluorescence microCT (computed tomography) is a novel technique that allows non-destructive determination of the 3D distribution of chemical elements inside a sample. This is especially important in samples for which sectioning is undesirable either due to the risk of contamination or the requirement for further analysis by different characterization techniques. Developments made by third generation synchrotron facilities and laboratory X-ray focusing systems have made these kinds of measurements more attractive by significantly reducing scan times and beam size. First results from the x-ray fluorescence microCT experiments performed at SSRL beamline 6-2 are reported here. Beamline 6-2 is a 54 pole wiggler that uses a two mirror optical system for focusing the x-rays onto a virtual source slit which is then reimaged with a set of KB mirrors to a (2 x 4) {micro}{sup 2} beam spot. An energy dispersive fluorescence detector is located in plane at 90 degrees to the incident beam to reduce the scattering contribution. A PIN diode located behind the sample simultaneously measures the x-ray attenuation in the sample. Several porous micrometeorite samples were measured and the reconstructed element density distribution including self-absorption correction is presented. Ultimately, this system will be used to analyze particles from the coma of comet Wild-2 and fresh interstellar dust particles both of which were collected during the NASA Stardust mission.

  16. TU-A-9A-09: Proton Beam X-Ray Fluorescence CT

    SciTech Connect

    Bazalova, M; Ahmad, M; Fahrig, R; Xing, L

    2014-06-15

    Purpose: To evaluate x-ray fluorescence computed tomography induced with proton beams (pXFCT) for imaging of gold contrast agent. Methods: Proton-induced x-ray fluorescence was studied by means of Monte Carlo (MC) simulations using TOPAS, a MC code based on GEANT4. First, proton-induced K-shell and L-shell fluorescence was studied as a function of proton beam energy and 1) depth in water and 2) size of contrast object. Second, pXFCT images of a 2-cm diameter cylindrical phantom with four 5- mm diameter contrast vials and of a 20-cm diameter phantom with 1-cm diameter vials were simulated. Contrast vials were filled with water and water solutions with 1-5% gold per weight. Proton beam energies were varied from 70-250MeV. pXFCT sinograms were generated based on the net number of gold K-shell or L-shell x-rays determined by interpolations from the neighboring 0.5keV energy bins of spectra collected with an idealized 4π detector. pXFCT images were reconstructed with filtered-back projection, and no attenuation correction was applied. Results: Proton induced x-ray fluorescence spectra showed very low background compared to x-ray induced fluorescence. Proton induced L-shell fluorescence had a higher cross-section compared to K-shell fluorescence. Excitation of L-shell fluorescence was most efficient for low-energy protons, i.e. at the Bragg peak. K-shell fluorescence increased with increasing proton beam energy and object size. The 2% and 5% gold contrast vials were accurately reconstructed in K-shell pXFCT images of both the 2-cm and 20-cm diameter phantoms. Small phantom L-shell pXFCT image required attenuation correction and had a higher sensitivity for 70MeV protons compared to 250MeV protons. With attenuation correction, L-shell pXFCT might be a feasible option for imaging of small size (∼2cm) objects. Imaging doses for all simulations were 5-30cGy. Conclusion: Proton induced x-ray fluorescence CT promises to be an alternative quantitative imaging technique to

  17. Detection limits for actinides in a monochromatic, wavelength-dispersive x-ray fluorescence instrument

    SciTech Connect

    Collins, Michael L; Havrilla, George J

    2009-01-01

    Recent developments in x-ray optics have made it possible to examine the L x-rays of actinides using doubly-curved crystals in a bench-top device. A doubly-curved crystal (DCC) acts as a focusing monochromatic filter for polychromatic x-rays. A Monochromatic, Wavelength-Dispersive X-Ray Fluorescence (MWDXRF) instrument that uses DCCs to measure Cm and Pu in reprocessing plant liquors was proposed in 2007 by the authors at Los Alamos National Laboratory. A prototype design of this MWDXRF instrument was developed in collaboration with X-ray Optical Systems Inc. (XOS), of East Greenbush, New York. In the MWDXRF instrument, x-rays from a Rhodium-anode x-ray tube are passed through a primary DCC to produce a monochromatic beam of 20.2-keV photons. This beam is focused on a specimen that may contain actinides. The 20.2-keV interrogating beam is just above the L3 edge of Californium; each actinide (with Z = 90 to 98) present in the specimen emits characteristic L x-rays as the result of L3-shell vacancies. In the LANL-XOS prototype MWDXRf, these x-rays enter a secondary DCC optic that preferentially passes 14.961-keV photons, corresponding to the L-alpha-1 x-ray peak of Curium. In the present stage of experimentation, Curium-bearing specimens have not been analyzed with the prototype MWDXRF instrument. Surrogate materials for Curium include Rubidium, which has a K-beta-l x-ray at 14.961 keV, and Yttrium, which has a K-alpha-1 x-ray at 14.958 keV. In this paper, the lower limit of detection for Curium in the LANL-XOS prototype MWDXRF instrument is estimated. The basis for this estimate is described, including a description of computational models and benchmarking techniques used. Detection limits for other actinides are considered, as well as future safeguards applications for MWDXRF instrumentation.

  18. First application of superconducting transition-edge sensor microcalorimeters to hadronic atom X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Okada, S.; Bennett, D. A.; Curceanu, C.; Doriese, W. B.; Fowler, J. W.; Gard, J. D.; Gustafsson, F. P.; Hashimoto, T.; Hayano, R. S.; Hirenzaki, S.; Hays-Wehle, J. P.; Hilton, G. C.; Ikeno, N.; Iliescu, M.; Ishimoto, S.; Itahashi, K.; Iwasaki, M.; Koike, T.; Kuwabara, K.; Ma, Y.; Marton, J.; Noda, H.; O'Neil, G. C.; Outa, H.; Reintsema, C. D.; Sato, M.; Schmidt, D. R.; Shi, H.; Suzuki, K.; Suzuki, T.; Swetz, D. S.; Tatsuno, H.; Uhlig, J.; Ullom, J. N.; Widmann, E.; Yamada, S.; Yamagata-Sekihara, J.; Zmeskal, J.

    2016-09-01

    High-resolution pionic atom X-ray spectroscopy was performed with an X-ray spectrometer based on a 240 pixel array of superconducting transition-edge sensor (TES) microcalorimeters at the πM1 beam line of the Paul Scherrer Institute. X-rays emitted by pionic carbon via the 4f→3d transition and the parallel 4d→3p transition were observed with a full width at half maximum energy resolution of 6.8 eV at 6.4 keV. The measured X-ray energies are consistent with calculated electromagnetic values which considered the strong interaction effect assessed via the Seki-Masutani potential for the 3p energy level, and favor the electronic population of two filled 1s electrons in the K-shell. Absolute energy calibration with an uncertainty of 0.1 eV was demonstrated under a high-rate hadron beam condition of 1.45 MHz. This is the first application of a TES spectrometer to hadronic atom X-ray spectroscopy and is an important milestone towards next-generation high-resolution kaonic atom X-ray spectroscopy.

  19. The application of a microstrip gas counter to energy-dispersive x-ray fluorescence analysis

    SciTech Connect

    Veloso, J.F.C.A.; Santos, J.M.F. dos; Conde, C.A.N.; Morgado, R.E.

    1996-07-01

    Performance characteristics of a microstrip gas counter operated as a x-ray fluorescence spectrometer are reported. Gas amplification as a function of microstrip anode-cathode voltage was measured, and the breakdown threshold voltage was determined in pure xenon. The detector temporal stability and the effect of gas purity were assessed. Energy resolution and linearity, detection efficiency, and uniformity of spatial response in the 2- to 60-keV x-ray energy range were determined from the pulse-height distributions of the fluorescence x-ray spectra induced in a variety of single- and multi-element sample materials. Energy resolution similar to conventional proportional counters was achieved at 6 keV.

  20. Application of a high-resolution x-ray fluorescence analyzer.

    SciTech Connect

    Adams, B. W.; Attenkofer, K.; Experimental Facilities Division

    2006-01-01

    We have developed a high resolution x-ray fluorescence analyzer based on the principle of active optics. It combines a resolution of ca. 5 eV with a tunability over several keV and a wide solid-angle coverage (ca. 2 by 5 degrees). To date, this analyzer has been used in near-edge spectroscopy of gallium in GaAs, and for the detection and chemical speciation of trace amounts platinum in soot from an diesel engine. The latter application illustrates the use of the analyzer to enhance the signal-to-background ratio in trace-element x-ray fluorescence analysis. The analyzer is shown schematically in Fig. 1. In it, a strip of silicon is bent by an axial force from two pushers at its ends, and eight correctors act from above to bring the shape of the bent crystal to approximate a logarithmic spiral. A more detailed description of the device, its underlying theory, and adjustment procedures may be found elsewhere. The sample consisted of soot collected from the exhaust of a diesel engine burning a fuel with a platinum-based additive that was tested for the purpose of facilitating clean combustion. The concentration of platinum in the soot was about 100 ppm, and the chemical speciation (oxidation state, dispersed or in the form of nanoparticles, etc.) was unknown. A small speck of this soot containing 10{sup 12} to 10{sup 13} atoms was placed into the x-ray beam of the 11-ID-D station of the APS. The incident photon energy was scanned over the Pt L{sub 3} edge, and the Pt L{sub {alpha}1} fluorescence was detected using two silicon drift detectors (Vortex), one directly and one with the analyzer. The purpose of the analyzer in this application was to enhance the energy resolution by a factor of about 50 (250 eV for the drift detector, 5 eV for the analyzer), and thus reduce the background of elastically or Compton-scattered photons, while keeping the fluorescent line. Whereas the detector with the analyzer recorded a clear signature of platinum in the form of an absorption

  1. Quantitative X-ray fluorescence analysis of samples of less than `infinite thickness': Difficulties and possibilities

    NASA Astrophysics Data System (ADS)

    Sitko, Rafał

    2009-11-01

    X-ray fluorescence spectrometry due to its nondestructive nature is widely applied in analysis of single layers and multiple layer films (e.g. semiconductors, electrooptic and solar cell devices, coatings, corrosion and paint layers), individual particles (airborne, fly ash, gunshot residue particles, etc.), art and archeological objects (manuscripts, paintings, icons) and many others. Quantitative analysis of these materials, frequently classified as samples of less than infinite thickness (thin or intermediate-thickness samples), required applying adequate matrix correction methods taking into account complex dependence of analyte fluorescent radiation intensity on full matrix composition and sample thickness. In this article, the matrix correction methods including fundamental parameters, Monte Carlo simulations, influence coefficients algorithms and methods based on X-ray transmission measurements are reviewed. The difficulties in the analysis of single layer and multiple layer films and the accuracy of fundamental parameter methods in simultaneous determination of their thickness and composition are discussed. The quantitative analysis of individual particles and inhomogeneous and/or complex structure materials using fundamental parameter and Monte Carlo simulation methods in micro-beam X-ray fluorescence spectrometry are also reviewed. Some references are devoted to the analysis of light matrix samples, e.g. geological, environmental and biological samples, in which undetectable low-Z elements are present (so-called 'dark matrix') using backscattered fundamental parameter methods. Since the samples of less than infinite thickness are partially transparent for X-ray beams, the transmission measurements present possibilities that are unattainable for bulk samples. Thus, the emission-transmission method and also new instruments allowing measurements of the primary X-ray beam transmitted through the sample together with measurements of X-ray fluorescence

  2. Atomic physics with hard X-rays from high brilliance synchrotron light sources

    SciTech Connect

    Southworth, S.; Gemmell, D.

    1996-08-01

    A century after the discovery of x rays, the experimental capability for studying atomic structure and dynamics with hard, bright synchrotron radiation is increasing remarkably. Tempting opportunities arise for experiments on many-body effects, aspects of fundamental photon-atom interaction processes, and relativistic and quantum-electrodynamic phenomena. Some of these possibilities are surveyed in general terms.

  3. Use of a Superconducting Tunnel Junction for X-Ray Fluorescence Spectroscopy

    SciTech Connect

    Hiller, Lawrence James

    2001-03-06

    A superconducting tunnel junction (STJ) in combination with a superconducting absorber of radiation may function as a highly resolving x-ray spectrometer. Electronic excitations, or quasiparticles, are created when a superconductor absorbs an x ray and are detected as an excess tunnel current through the junction. The number of quasiparticles created and the magnitude of the excess current is proportional to the energy of the absorbed x ray. This is similar to existing semiconductor-based spectrometers that measure electron-hole pairs, but with 1000 times more excitations. The energy measurement therefore can be up to 30 times more precise with a superconducting detector than with a semiconductor detector. This work describes the development and testing of an STJ spectrometer design for x-ray fluorescence applications. First, the basic principles of the STJ spectrometer are explained. This is followed by detailed simulations of the variance in the number of quasiparticles produced by absorption of an x ray. This variance is inherent in the detector and establishes an upper limit on the resolving power of the spectrometer. These simulations include effects due to the materials used in the spectrometer and to the multilayer structure of the device. Next, the spectrometer is characterized as functions of operating temperature, incident x-ray energy, and count rate. Many of these tests were performed with the spectrometer attached to a synchrotron radiation port. Finally, example x-ray fluorescence spectra of materials exposed to synchrotron radiation are presented. These materials are of interest to semiconductor processing and structural biology, two fields that will benefit immediately from the improved resolving power of the STJ spectrometer.

  4. Three-dimensional readout of flash x-ray images of living sperm in water by atomic-force microscopy.

    PubMed

    Tomie, T; Shimizu, H; Majima, T; Yamada, M; Kanayama, T; Kondo, H; Yano, M; Ono, M

    1991-05-03

    The imaging of living specimens in water by x-ray microscopy can be greatly enhanced with the use of an intense flash x-ray source and sophisticated technologies for reading x-ray images. A subnanosecond [corrected] x-ray pulse from a laser-produced plasma was used to record the x-ray image of living sea urchin sperm in an x-ray resist. The resist relief was visualized at high resolution by atomic-force microscopy. Internal structure of the sperm head was evident, and the carbon density in a flagellum was estimated from the relief height.

  5. Quantitative measurement of PM10 by means of X-ray fluorescence spectra

    NASA Astrophysics Data System (ADS)

    Busetto, E.; Peloi, M.; Rebuffi, L.; Tefouet Kana, E.

    2013-05-01

    We developed an automatic device able to sample and analyze in situ and in real time airborne particulate matter (PM) using the X-ray fluorescence of the chemical species layered on a filter, having atomic numbers between 19 (Potassium) and 82 (Lead). Furthermore, we developed a calibration technique, which gives the parameters for real time automatic determination of the absolute mass of the chemical species present on the sample, with a sensitivity varying from 1 to 100 μg per sample. Our system could represent a simpler alternative to the complex and sophisticated laboratory measurements, such as Inductively Coupled Plasma Mass Spectrometry (ICP-MS) or Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES), officially used by environmental agencies. A 6 month in-situ test, carried out in collaboration with the local Regional Environmental Agency, showed that our system gives results comparable with the ones obtained using existing techniques, but with smaller errors. The methodology developed has been submitted for a patent.

  6. Development of an X-ray fluorescence holographic measurement system for protein crystals

    NASA Astrophysics Data System (ADS)

    Sato-Tomita, Ayana; Shibayama, Naoya; Happo, Naohisa; Kimura, Koji; Okabe, Takahiro; Matsushita, Tomohiro; Park, Sam-Yong; Sasaki, Yuji C.; Hayashi, Kouichi

    2016-06-01

    Experimental procedure and setup for obtaining X-ray fluorescence hologram of crystalline metalloprotein samples are described. Human hemoglobin, an α2β2 tetrameric metalloprotein containing the Fe(II) heme active-site in each chain, was chosen for this study because of its wealth of crystallographic data. A cold gas flow system was introduced to reduce X-ray radiation damage of protein crystals that are usually fragile and susceptible to damage. A χ-stage was installed to rotate the sample while avoiding intersection between the X-ray beam and the sample loop or holder, which is needed for supporting fragile protein crystals. Huge hemoglobin crystals (with a maximum size of 8 × 6 × 3 mm3) were prepared and used to keep the footprint of the incident X-ray beam smaller than the sample size during the entire course of the measurement with the incident angle of 0°-70°. Under these experimental and data acquisition conditions, we achieved the first observation of the X-ray fluorescence hologram pattern from the protein crystals with minimal radiation damage, opening up a new and potential method for investigating the stereochemistry of the metal active-sites in biomacromolecules.

  7. Laboratory Setup for Scanning-Free Grazing Emission X-ray Fluorescence.

    PubMed

    Baumann, J; Herzog, C; Spanier, M; Grötzsch, D; Lühl, L; Witte, K; Jonas, A; Günther, S; Förste, F; Hartmann, R; Huth, M; Kalok, D; Steigenhöfer, D; Krämer, M; Holz, T; Dietsch, R; Strüder, L; Kanngießer, B; Mantouvalou, I

    2017-02-07

    Grazing incidence and grazing emission X-ray fluorescence spectroscopy (GI/GE-XRF) are techniques that enable nondestructive, quantitative analysis of elemental depth profiles with a resolution in the nanometer regime. A laboratory setup for soft X-ray GEXRF measurements is presented. Reasonable measurement times could be achieved by combining a highly brilliant laser produced plasma (LPP) source with a scanning-free GEXRF setup, providing a large solid angle of detection. The detector, a pnCCD, was operated in a single photon counting mode in order to utilize its energy dispersive properties. GEXRF profiles of the Ni-Lα,β line of a nickel-carbon multilayer sample, which displays a lateral (bi)layer thickness gradient, were recorded at several positions. Simulations of theoretical profiles predicted a prominent intensity minimum at grazing emission angles between 5° and 12°, depending strongly on the bilayer thickness of the sample. This information was used to retrieve the bilayer thickness gradient. The results are in good agreement with values obtained by X-ray reflectometry, conventional X-ray fluorescence and transmission electron microscopy measurements and serve as proof-of-principle for the realized GEXRF setup. The presented work demonstrates the potential of nanometer resolved elemental depth profiling in the soft X-ray range with a laboratory source, opening, for example, the possibility of in-line or even in situ process control in semiconductor industry.

  8. Determining the Conformation of an Adsorbed Br-PEG-Peptide by Long Period X-ray Standing Wave Fluorescence

    PubMed Central

    Crot, Carrie A.; Wu, Chunping; Schlossman, Mark L.; Trainor, Thomas P.; Eng, Peter J.; Hanley, Luke

    2008-01-01

    Long period x-ray standing wave fluorescence (XSW) and x-ray reflectivity techniques are employed to probe the conformation of a Br-polyethylene glycol (PEG)-peptide adsorbate at the hydrated interface of a polystyrene substrate. The Br atom on this Br-PEG-peptide construct serves as a marker atom allowing determination by XSW of its position and distribution with respect to the adsorption surface with angstrom resolution. Adsorption occurs on native or ion beam modified polystyrene films that are spin coated onto a Si substrate and display either nonpolar or polar surfaces, respectively. A compact, oriented monolayer of Br-PEG-peptide can be formed with the peptide end adsorbed onto the polar surface and the PEG end terminating with the Br tag extending into the aqueous phase. The 108 – 141 Å distance of the Br atom from the polystyrene surface in this oriented monolayer is similar to the estimated ~150 Å length of the extended Br-PEG-peptide. This Br-polystyrene distance depends upon adsorption time and surface properties prior to adsorption. Incomplete multilayers form on the polar surface after sufficient adsorption time elapses. By contrast, adsorption onto the nonpolar surface is submonolayer, patchy, and highly disordered with an isotropic Br distribution. Overall, this combination of x-ray surface scattering techniques with a novel sample preparation strategy has several advantages as a real space probe of adsorbed or covalently bound biomolecules at the liquid-solid interface. PMID:16089398

  9. Atom Specific Ultrafast Surface Chemistry using a Soft X-ray Laser

    NASA Astrophysics Data System (ADS)

    Nilsson, Anders

    2014-03-01

    Catalysis is central for many chemical energy transformations that occur at interfaces. One of the dreams is to follow catalytic reactions in real time from reactants over various intermediates to products. The prospective for the study of chemical reactions on surfaces using X-ray free-electron lasers (Linac Coherent Light Source, or LCLS, at SLAC National Accelerator Laboratory) will be presented. We induced the hot electron and phonon mediated excitation of adsorbates on Ru(0001) with synchronized excitation by a femtosecond optical laser pulse. We have followed the ultrafast evolution of the bond distortions, weakening and breaking, using x-ray absorption spectroscopy and x ray emission spectroscopy resonantly tuned to the oxygen core level with ultrashort x-ray pulses delivered from LCLS. We can directly follow the time evolution of the molecular orbitals in an atom-specific way on a subpicosecond timescale. Three examples will be shown CO desorption, Oxygen activation and CO oxidation on Ru(0001).

  10. The use of a mercuric iodide detector for X-ray fluorescence analysis in archaeometry

    NASA Astrophysics Data System (ADS)

    Cesareo, R.; Gigante, G. E.; Iwanczyk, J. S.; Dabrowski, A.

    1992-11-01

    For about two decades, energy dispersive X-ray fluorescence (EDXRF) has been employed in Rome for the analysis of works of art. A short history of the applications of EDXRF to paintings and alloys is presented. Finally, the usefulness of mercuric iodide room-temperature semiconductor detectors in this field is shown.

  11. Rapid screening for zinc deficiency using portable x-ray fluorescence in fingernails

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Elemental composition of fingernails is a useful indicator of micronutrient status and may reflect an individual’s intake over time. Our objective was to determine if portable X-ray fluorescence (XRF) is a viable method to assess zinc content in fingernails in the field. Human fingernail samples ran...

  12. Simultaneous cryo X-ray ptychographic and fluorescence microscopy of green algae

    PubMed Central

    Deng, Junjing; Vine, David J.; Chen, Si; Nashed, Youssef S. G.; Jin, Qiaoling; Phillips, Nicholas W.; Peterka, Tom; Ross, Rob; Vogt, Stefan; Jacobsen, Chris J.

    2015-01-01

    Trace metals play important roles in normal and in disease-causing biological functions. X-ray fluorescence microscopy reveals trace elements with no dependence on binding affinities (unlike with visible light fluorophores) and with improved sensitivity relative to electron probes. However, X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular material. Here we show that X-ray ptychography can be combined with fluorescence to image both cellular structure and trace element distribution in frozen-hydrated cells at cryogenic temperatures, with high structural and chemical fidelity. Ptychographic reconstruction algorithms deliver phase and absorption contrast images at a resolution beyond that of the illuminating lens or beam size. Using 5.2-keV X-rays, we have obtained sub–30-nm resolution structural images and ∼90-nm–resolution fluorescence images of several elements in frozen-hydrated green algae. This combined approach offers a way to study the role of trace elements in their structural context. PMID:25675478

  13. Analysis of tincal ore waste by energy dispersive X-ray fluorescence (EDXRF) Technique

    NASA Astrophysics Data System (ADS)

    Kalfa, Orhan Murat; Üstündağ, Zafer; Özkırım, Ilknur; Kagan Kadıoğlu, Yusuf

    2007-01-01

    Etibank Borax Plant is located in Kırka-Eskişehir, Turkey. The borax waste from this plant was analyzed by means of energy dispersive X-ray fluorescence (EDXRF). The standard addition method was used for the determination of the concentration of Al, Fe, Zn, Sn, and Ba. The results are presented and discussed in this paper.

  14. Filter-fluorescer measurement of low-voltage simulator x-ray energy spectra

    SciTech Connect

    Baldwin, G.T.; Craven, R.E.

    1986-01-01

    X-ray energy spectra of the Maxwell Laboratories MBS and Physics International Pulserad 737 were measured using an eight-channel filter-fluorescer array. The PHOSCAT computer code was used to calculate channel response functions, and the UFO code to unfold spectrum.

  15. Energy-Dispersive X-Ray Fluorescence Spectrometry: A Long Overdue Addition to the Chemistry Curriculum

    ERIC Educational Resources Information Center

    Palmer, Peter T.

    2011-01-01

    Portable Energy-Dispersive X-Ray Fluorescence (XRF) analyzers have undergone significant improvements over the past decade. Salient advantages of XRF for elemental analysis include minimal sample preparation, multielement analysis capabilities, detection limits in the low parts per million (ppm) range, and analysis times on the order of 1 min.…

  16. Determination of rhenium in molybdenite by X-ray fluorescence. A combined chemical-spectrometric technique

    USGS Publications Warehouse

    Solt, M.W.; Wahlberg, J.S.; Myers, A.T.

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 ??g of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. ?? 1969.

  17. Radiochemical Analysis by High Sensitivity Micro X-Ray Fluorescence Detection

    SciTech Connect

    Ning Gao

    2006-05-12

    The primary objective of the project was to develop a novel dual-optic x-ray fluorescence instrument capable of doing radiochemical analysis of high-level radioactive wastes at DOE sites such as Savannah River Site and Hanford Site.

  18. CHARACTERIZATION OF CHROMIUM-CONTAMINATED SOILS USING FIELD-PORTABLE X-RAY FLUORESCENCE

    EPA Science Inventory

    A detailed characterization of the underlying and adjacent soils near a chrome plating shop utilized field-portable X- ray fluorescence (XRF) as a screening tool. XRF permitted real-time acquisition of estimates for total metal content of soils. A trailer-mounted soil coring unit...

  19. ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT - FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER - HNU SYSTEMS, SEFA-P

    EPA Science Inventory

    In April 1995, the Environmental Protection Agency (EPA) conducted a demonstration of field portable X-ray fluorescence (FPXRF) Analyzers. The primary objectives of this demonstration were (1) to determine how well FPXRF analyzers perform in comparison to a standard reference m...

  20. ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT - FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER - SCITEC, MAP SPECTRUM ANALYZER

    EPA Science Inventory

    In April 1995, the U.S. Environmental Protection Agency (EPA) sponsored a demonstration of field portable X-ray fluorescence (FPXRF) analyzers. The primary objectives of this demonstration were (1) to determine how well FPXRF analyzers perform in comparison to standard reference...

  1. Americium characterization by X-ray fluorescence and absorption spectroscopy in plutonium uranium mixed oxide

    SciTech Connect

    Degueldre, Claude Cozzo, Cedric; Martin, Matthias; Grolimund, Daniel; Mieszczynski, Cyprian

    2013-06-01

    Plutonium uranium mixed oxide (MOX) fuels are currently used in nuclear reactors. The actinides in these fuels need to be analyzed after irradiation for assessing their behaviour with regard to their environment and the coolant. In this work the study of the atomic structure and next-neighbour environment of Am in the (Pu,U)O₂ lattice in an irradiated (60 MW d kg⁻¹) MOX sample was performed employing micro-X-ray fluorescence (µ-XRF) and micro-X-ray absorption fine structure (µ-XAFS) spectroscopy. The chemical bonds, valences and stoichiometry of Am (~0.66 wt%) are determined from the experimental data gained for the irradiated fuel material examined in its peripheral zone (rim) of the fuel. In the irradiated sample Am builds up as Am³⁺ species within an [AmO₈]¹³⁻ coordination environment (e.g. >90%) and no (<10%) Am(IV) or (V) can be detected in the rim zone. The occurrence of americium dioxide is avoided by the redox buffering activity of the uranium dioxide matrix. - Graphical abstract: Americium LIII XAFS spectra recorded for the irradiated MOX sub-sample in the rim zone for a 300 μm×300 μm beam size area investigated over six scans of 4 h. The records remain constant during multi-scan. The analysis of the XAFS signal shows that Am is found as trivalent in the UO₂ matrix. This analytical work shall open the door of very challenging analysis (speciation of fission product and actinides) in irradiated nuclear fuels. - Highlights: • Americium was characterized by microX-ray absorption spectroscopy in irradiated MOX fuel. • The americium redox state as determined from XAS data of irradiated fuel material was Am(III). • In the sample, the Am³⁺ face an AmO₈¹³⁻coordination environment in the (Pu,U)O₂ matrix. • The americium dioxide is reduced by the uranium dioxide matrix.

  2. First demonstration of multiplexed X-ray fluorescence computed tomography (XFCT) imaging.

    PubMed

    Kuang, Yu; Pratx, Guillem; Bazalova, Magdalena; Meng, Bowen; Qian, Jianguo; Xing, Lei

    2013-02-01

    Simultaneous imaging of multiple probes or biomarkers represents a critical step toward high specificity molecular imaging. In this work, we propose to utilize the element-specific nature of the X-ray fluorescence (XRF) signal for imaging multiple elements simultaneously (multiplexing) using XRF computed tomography (XFCT). A 5-mm-diameter pencil beam produced by a polychromatic X-ray source (150 kV, 20 mA) was used to stimulate emission of XRF photons from 2% (weight/volume) gold (Au), gadolinium (Gd), and barium (Ba) embedded within a water phantom. The phantom was translated and rotated relative to the stationary pencil beam in a first-generation CT geometry. The X-ray energy spectrum was collected for 18 s at each position using a cadmium telluride detector. The spectra were then used to isolate the K shell XRF peak and to generate sinograms for the three elements of interest. The distribution and concentration of the three elements were reconstructed with the iterative maximum likelihood expectation maximization algorithm. The linearity between the XFCT intensity and the concentrations of elements of interest was investigated. We found that measured XRF spectra showed sharp peaks characteristic of Au, Gd, and Ba. The narrow full-width at half-maximum (FWHM) of the peaks strongly supports the potential of XFCT for multiplexed imaging of Au, Gd, and Ba ( FWHM(Au,Kα1) = 0.619 keV, FWHM(Au,Kα2)=1.371 keV , FWHM(Gd,Kα)=1.297 keV, FWHM(Gd,Kβ)=0.974 keV , FWHM(Ba,Kα)=0.852 keV, and FWHM(Ba,Kβ)=0.594 keV ). The distribution of Au, Gd, and Ba in the water phantom was clearly identifiable in the reconstructed XRF images. Our results showed linear relationships between the XRF intensity of each tested element and their concentrations ( R(2)(Au)=0.944 , R(Gd)(2)=0.986, and R(Ba)(2)=0.999), suggesting that XFCT is capable of quantitative imaging. Finally, a transmission CT image was obtained to show the potential of the approach for providing attenuation correction

  3. Full Field X-Ray Fluorescence Imaging Using Micro Pore Optics for Planetary Surface Exploration

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Blake, D. F.; Gailhanou, M.; Walter, P.; Schyns, E.; Marchis, F.; Thompson, K.; Bristow, T.

    2016-01-01

    Many planetary surface processes leave evidence as small features in the sub-millimetre scale. Current planetary X-ray fluorescence spectrometers lack the spatial resolution to analyse such small features as they only provide global analyses of areas greater than 100 mm(exp 2). A micro-XRF spectrometer will be deployed on the NASA Mars 2020 rover to analyse spots as small as 120m. When using its line-scanning capacity combined to perpendicular scanning by the rover arm, elemental maps can be generated. We present a new instrument that provides full-field XRF imaging, alleviating the need for precise positioning and scanning mechanisms. The Mapping X-ray Fluorescence Spectrometer - "Map-X" - will allow elemental imaging with approximately 100µm spatial resolution and simultaneously provide elemental chemistry at the scale where many relict physical, chemical and biological features can be imaged in ancient rocks. The arm-mounted Map-X instrument is placed directly on the surface of an object and held in a fixed position during measurements. A 25x25 mm(exp 2) surface area is uniformly illuminated with X-rays or alpha-particles and gamma-rays. A novel Micro Pore Optic focusses a fraction of the emitted X-ray fluorescence onto a CCD operated at a few frames per second. On board processing allows measuring the energy and coordinates of each X-ray photon collected. Large sets of frames are reduced into 2d histograms used to compute higher level data products such as elemental maps and XRF spectra from selected regions of interest. XRF spectra are processed on the ground to further determine quantitative elemental compositions. The instrument development will be presented with an emphasis on the characterization and modelling of the X-ray focussing Micro Pore Optic. An outlook on possible alternative XRF imaging applications will be discussed.

  4. X-ray fluorescence microtomography of SiC shells

    SciTech Connect

    Ice, G.E.; Chung, J.S.; Nagedolfeizi, M.

    1997-04-01

    TRISCO coated fuel particles contain a small kernel of nuclear fuel encapsulated by alternating layers of C and SiC. The TRISCO coated fuel particle is used in an advanced fuel designed for passive containment of the radioactive isotopes. The SiC layer provides the primary barrier for radioactive elements in the kernel. The effectiveness of this barrier layer under adverse conditions is critical to containment. The authors have begun the study of SiC shells from TRISCO fuel. They are using the fluorescent microprobe beamline 10.3.1. The shells under evaluation include some which have been cycled through a simulated core melt-down. The C buffer layers and nuclear kernels of the coated fuel have been removed by laser drilling through the SiC and then exposing the particle to acid. Elements of interest include Ru, Sb, Cs, Ce and Eu. The radial distribution of these elements in the SiC shells can be attributed to diffusion of elements in the kernel during the melt-down. Other elements in the shells originate during the fabrication of the TRISCO particles.

  5. A High-Speed Detector System for X-ray Fluorescence Microprobes.

    SciTech Connect

    Siddons,P.D.; Dragone, A.; De Geronimo, g.; Kuczewski, A.; Kuczewski, J.; O

    2006-10-29

    We have developed a high-speed system for collecting x-ray fluorescence microprobe data, based on ASICs developed at BNL and high-speed processors developed by CSIRO. The system can collect fluorescence data in a continuous raster scan mode, and present elemental images in real time using Ryan's Dynamic Analysis algorithm. We will present results from a 32-element prototype array illustrating the concept. The final instrument will have 384 elements arranged in a square array around a central hole.

  6. Pulsed fluorescent x-ray system with on-line digitizer and data processor

    SciTech Connect

    Berzins, G.J.; Valencia, J.E.; Gutierrez, J.W.; McGirt, F.; Moore, K.R.

    1984-12-01

    A pulsed source of monoenergetic x rays has been constructed for applications in which a narrow energy band and a short burst are both important. The radiation source is a high-purity, selectable foil that emits fluorescent x rays upon excitation by a bremsstrahlung pulse. A digitizer and a microcomputer are integrated into the system to aid operation and data processing. A general description, the more important system characteristics, and a few examples of applications are given. 7 references, 10 figures, 6 tables.

  7. Spatially resolved density and ionization measurements of shocked foams using x-ray fluorescence

    DOE PAGES

    MacDonald, M. J.; Keiter, P. A.; Montgomery, D. S.; ...

    2016-09-22

    We present experiments at the Trident laser facility demonstrating the use of x-ray fluorescence (XRF) to simultaneously measure density, ionization state populations, and electron temperature in shocked foams. An imaging x-ray spectrometer was used to obtain spatially-resolved measurements of Ti K-more » $$\\alpha$$ emission. Density profiles were measured from K-$$\\alpha$$ intensity. Ti ionization state distributions and electron temperatures were inferred by fitting K-$$\\alpha$$ spectra to spectra from CRETIN simulations. This study shows that XRF provides a powerful tool to complement other diagnostics to make equation of state measurements of shocked materials containing a suitable tracer element.« less

  8. Spatially resolved density and ionization measurements of shocked foams using x-ray fluorescence

    SciTech Connect

    MacDonald, M. J.; Keiter, P. A.; Montgomery, D. S.; Scott, H. A.; Biener, M. M.; Fein, J. R.; Fournier, K. B.; Gamboa, E. J.; Kemp, G. E.; Klein, S. R.; Kuranz, C. C.; LeFevre, H. J.; Manuel, M. J. -E.; Wan, W. C.; Drake, R. P.

    2016-09-22

    We present experiments at the Trident laser facility demonstrating the use of x-ray fluorescence (XRF) to simultaneously measure density, ionization state populations, and electron temperature in shocked foams. An imaging x-ray spectrometer was used to obtain spatially-resolved measurements of Ti K-$\\alpha$ emission. Density profiles were measured from K-$\\alpha$ intensity. Ti ionization state distributions and electron temperatures were inferred by fitting K-$\\alpha$ spectra to spectra from CRETIN simulations. This study shows that XRF provides a powerful tool to complement other diagnostics to make equation of state measurements of shocked materials containing a suitable tracer element.

  9. An x-ray setup to investigate the atomic order of confined liquids in slit geometry

    SciTech Connect

    Lippmann, M.; Ehnes, A.; Seeck, O. H.

    2014-01-15

    A setup has been designed to investigate thin films of confined liquids with the use of X-ray scattering methods. The confinement is realized between the flat culets of a pair of diamonds by positioning and orienting the lower diamond with nanometer and micro radian accuracy. We routinely achieve gaps between 5 and 50 nm at culet diameters of 200 μm. With this setup and a micro focused X-ray beam we have investigated the in-plane and the out-off-plane atomic order of benzene with atomic resolution.

  10. All dielectric hard x-ray mirror by atomic layer deposition

    NASA Astrophysics Data System (ADS)

    Szeghalmi, Adriana; Senz, Stephan; Bretschneider, Mario; Gösele, Ulrich; Knez, Mato

    2009-03-01

    Mirrors consisting of Al2O3 and Ta2O5 (˜2 nm film thickness) nanolaminates for hard x-ray wavelengths were produced by atomic layer deposition and characterized. Atomic force microscopy and transmission electron microscopy (TEM) proved extremely smooth surfaces of the mirrors, which are critical for highest reflectance. TEM images showed sharp interfaces between the oxides. The experimental x-ray reflectivity data were theoretically modeled and indicated minimal random thickness variations in the individual layers. Additionally, a depth graded sample with a total thickness of ˜4 μm for focusing applications in transmission (Laue) geometry and capillaries was coated.

  11. An x-ray setup to investigate the atomic order of confined liquids in slit geometry.

    PubMed

    Lippmann, M; Ehnes, A; Seeck, O H

    2014-01-01

    A setup has been designed to investigate thin films of confined liquids with the use of X-ray scattering methods. The confinement is realized between the flat culets of a pair of diamonds by positioning and orienting the lower diamond with nanometer and micro radian accuracy. We routinely achieve gaps between 5 and 50 nm at culet diameters of 200 μm. With this setup and a micro focused X-ray beam we have investigated the in-plane and the out-off-plane atomic order of benzene with atomic resolution.

  12. Moseley's Work on X-Rays and Atomic Number.

    ERIC Educational Resources Information Center

    Haigh, C. W.

    1995-01-01

    Highlights the connection between the achievements of Moseley and the spectrum of the hydrogen atom, the Bohr theory, and Slater's rules for screening constants. Uses modern data to show that Moseley's equation is actually an approximation and discusses the significance of this fact. (JRH)

  13. Molar concentration from sequential 2-D water-window X-ray ptychography and X-ray fluorescence in hydrated cells

    PubMed Central

    Jones, M. W. M.; Elgass, K. D.; Junker, M. D.; de Jonge, M. D.; van Riessen, G. A.

    2016-01-01

    Recent developments in biological X-ray microscopy have allowed structural information and elemental distribution to be simultaneously obtained by combining X-ray ptychography and X-ray fluorescence microscopy. Experimentally, these methods can be performed simultaneously; however, the optimal conditions for each measurement may not be compatible. Here, we combine two distinct measurements of ultrastructure and elemental distribution, with each measurement performed under optimised conditions. By combining optimised ptychography and fluorescence information we are able to determine molar concentrations from two-dimensional images, allowing an investigation into the interactions between the environment sensing filopodia in fibroblasts and extracellular calcium. Furthermore, the biological ptychography results we present illustrate a point of maturity where the technique can be applied to solve significant problems in structural biology. PMID:27067957

  14. Fluorescence imaging as a diagnostic of M-band x-ray drive condition in hohlraum with fluorescent Si targets

    NASA Astrophysics Data System (ADS)

    Li, Qi; Hu, Zhimin; Yao, Li; Huang, Chengwu; Yuan, Zheng; Zhao, Yang; Xiong, Gang; Qing, Bo; Lv, Min; Zhu, Tuo; Deng, Bo; Li, Jin; Wei, Minxi; Zhan, Xiayu; Li, Jun; Yang, Yimeng; Su, Chunxiao; Yang, Guohong; Zhang, Jiyan; Li, Sanwei; Yang, Jiamin; Ding, Yongkun

    2017-01-01

    Fluorescence imaging of surrogate Si-doped CH targets has been used to provide a measurement for drive condition of high-energy x-ray (i.e. M-band x-ray) drive symmetry upon the capsule in hohlraum on Shenguang-II laser facility. A series of experiments dedicated to the study of photo-pumping and fluorescence effect in Si-plasma are presented. To investigate the feasibility of fluorescence imaging in Si-plasma, an silicon plasma in Si-foil target is pre-formed at ground state by the soft x-ray from a half-hohlraum, which is then photo-pumped by the K-shell lines from a spatially distinct laser-produced Si-plasma. The resonant Si photon pump is used to improve the fluorescence signal and cause visible image in the Si-foil. Preliminary fluorescence imaging of Si-ball target is performed in both Si-doped and pure Au hohlraum. The usual capsule at the center of the hohlraum is replaced with a solid Si-doped CH-ball (Si-ball). Since the fluorescence is proportional to the photon pump upon the Si-plasma, high-energy x-ray drive symmetry is equal to the fluorescence distribution of the Si-ball.

  15. Evaluation of fluorescent dye degradation indirectly induced by x-ray ionizing radiation.

    PubMed

    Benevides, Clayton Augusto; Duarte de Menezes, Frederico; de Araujo, Renato E

    2015-08-01

    This work evaluated the fluorescent dye degradation indirectly induced by ionizing radiation with high energy photons (50 keV). Aqueous gels of agarose with low concentrations of Rhodamine 6G and Fluorescein were submitted to doses of x-ray radiation up to 200 Gy. The dye degradation was analyzed by fluorescence spectroscopy, using an excitation light-emitting diode with a peak wavelength of 462 nm. A rate equation model of fluorophores and radicals' species populations was developed to describe the degradation time behavior of the fluorescent solutions. The model suggests fluorescent dyes should be used in dosimetry.

  16. Characterization of the scale on oxidized Fe-Ni-Cr alloys using grazing emission x-ray fluorescence.

    SciTech Connect

    Koshelev, I.; Paulikas, A. P.; Beno, M.; Jennings, G.; Linton, J.; Uran, S.; Veal, B. W.; Materials Science Division

    2001-09-01

    Grazing emission X-ray fluorescence (GEXRF, or refracted X-ray fluorescence-RXF) has been used to characterize the oxide scale (predominately chromia) which formed on an alloy of 55Fe-25Cr-20Ni (wt%) after oxidation for 4 h at 750{sup o}C in O{sub 2}. Angle dependent X-ray emission spectra I({theta}) were acquired for three elements, Cr, Fe and Ni. The measured data were fit by adjusting scale parameters in the calculated spectra such that I({theta}) data were simultaneously fit for all three elements. It is shown that the calculated spectra are sensitive to scale thickness, to the Cr depletion zone that develops in the substrate at the scale-metal interface, and to the concentration of Fe and Ni atoms dissolved in the scale. The very demanding requirements imposed by simultaneously fitting all three measured I({theta}) curves provide a satisfactory determination of these scale parameters. The GEXRF measurements showed that the scale was about 0.5 {mu}m thick, with an underlying Cr depletion zone extending about 4 {mu}m (midpoint) into the substrate. The average Cr concentration in this depletion zone was reduced from the preoxidized value of 25 to 22.2 wt%. The scale contained about 2. 4 at% of Fe and less than 0.5 at% Ni. These measurements demonstrate that GEXRF can, in a single nondestructive measurement, provide key information needed to characterize a thermally grown chromia scale.

  17. Inorganic chemical investigation by X-ray fluorescence analysis - The Viking Mars Lander

    NASA Technical Reports Server (NTRS)

    Toulmin, P., III; Rose, H. J., Jr.; Baird, A. K.; Clark, B. C.; Keil, K.

    1973-01-01

    The inorganic chemical investigation experiment added in August 1972 to the Viking Lander scientific package uses an energy-dispersive X-ray fluorescence spectrometer in which four sealed, gas-filled proportional counters detect X-rays emitted from samples of the Martian surface materials irradiated by X-rays from radioisotope sources (Fe-55 and Cd-109). The instrument is inside the Lander body, and samples are to be delivered to it by the Viking Lander Surface Sampler. Instrument design is described along with details of the data processing and analysis procedures. The results of the investigation will characterize the surface materials of Mars as to elemental composition with accuracies ranging from a few tens of parts per million (at the trace-element level) to a few per cent (for major elements) depending on the element in question.

  18. Micro X-ray Fluorescence Imaging in a Tabletop Full Field-X-ray Fluorescence Instrument and in a Full Field-Particle Induced X-ray Emission End Station.

    PubMed

    Romano, Francesco Paolo; Caliri, Claudia; Cosentino, Luigi; Gammino, Santo; Mascali, David; Pappalardo, Lighea; Rizzo, Francesca; Scharf, Oliver; Santos, Hellen Cristine

    2016-10-08

    A full field-X-ray camera (FF-XRC) was developed for performing the simultaneous mapping of chemical elements with a high lateral resolution. The device is based on a conventional CCD detector coupled to a straight shaped polycapillary. Samples are illuminated at once with a broad primary beam that can consist of X-rays or charged particles in two different analytical setups. The characteristic photons induced in the samples are guided by the polycapillary to the detector allowing the elemental imaging without the need for scanning. A single photon counting detection operated in a multiframe acquisition mode and a processing algorithm developed for event hitting reconstruction have enabled one to use the CCD as a high energy resolution X-ray detector. A novel software with a graphical user interface (GUI) programmed in Matlab allows full control of the device and the real-time imaging with a region-of-interest (ROI) method. At the end of the measurement, the software produces spectra for each of the pixels in the detector allowing the application of a least-squares fitting with external analytical tools. The FF-XRC is very compact and can be installed in different experimental setups. This work shows the potentialities of the instrument in both a full field-micro X-ray fluorescence (FF-MXRF) tabletop device and in a full field-micro particle induced X-ray emission (FF-MPIXE) end-station operated with an external proton beam. Some examples of applications are given as well.

  19. Sub-micron Hard X-ray Fluorescence Imaging of Synthetic Elements

    PubMed Central

    Jensen, Mark P.; Aryal, Baikuntha P.; Gorman-Lewis, Drew; Paunesku, Tatjana; Lai, Barry; Vogt, Stefan; Woloschak, Gayle E.

    2013-01-01

    Synchrotron-based X-ray fluorescence microscopy (SXFM) using hard X-rays focused into sub-micron spots is a powerful technique for elemental quantification and mapping, as well as microspectroscopic measurement such as μ-XANES (X-ray absorption near edge structure). We have used SXFM to image and simultaneously quantify the transuranic element plutonium at the L3 or L2 edge as well as lighter biologically essential elements in individual rat pheochromocytoma (PC12) cells after exposure to the long-lived plutonium isotope 242Pu. Elemental maps reveal that plutonium localizes principally in the cytoplasm of the cells and avoids the cell nucleus, which is marked by the highest concentrations of phosphorus and zinc, under the conditions of our experiments. The minimum detection limit under typical acquisition conditions for an average 202 μm2 cell is 1.4 fg Pu/cell or 2.9 × 10−20 moles Pu/μm2, which is similar to the detection limit of K-edge SXFM of transition metals at 10 keV. Copper electron microscopy grids were used to avoid interference from gold X-ray emissions, but traces of strontium present in naturally occurring calcium can still interfere with plutonium detection using its Lα X-ray emission. PMID:22444530

  20. Soft-x-ray fluorescence study of buried silicides in antiferromagnetically coupled Fe/Si multilayers

    SciTech Connect

    Carlisle, J.A.; Chaiken, A.; Michel, R.P.

    1997-04-01

    Multilayer films made by alternate deposition of two materials play an important role in electronic and optical devices such as quantum-well lasers and x-ray mirrors. In addition, novel phenomena like giant magnetoresistance and dimensional crossover in superconductors have emerged from studies of multilayers. While sophisticated x-ray techniques are widely used to study the morphology of multilayer films, progress in studying the electronic structure has been slower. The short mean-free path of low-energy electrons severely limits the usefulness of photoemission and related electron free path of low-energy electrons severely limit spectroscopies for multilayer studies. Soft x-ray fluorescence (SXF) is a bulk-sensitive photon-in, photon-out method to study valence band electronic states. Near-edge x-ray absorption fine-structure spectroscopy (NEXAFS) measured with partial photon yield can give complementary bulk-sensitive information about unoccupied states. Both these methods are element-specific since the incident x-ray photons excite electrons from core levels. By combining NEXAFS and SXF measurements on buried layers in multilayers and comparing these spectra to data on appropriate reference compounds, it is possible to obtain a detailed picture of the electronic structure. Results are presented for a study of a Fe/Si multilayer system.

  1. Evaluation of different synchrotron beamline configurations for X-ray fluorescence analysis of environmental samples.

    PubMed

    Barberie, Sean R; Iceman, Christopher R; Cahill, Catherine F; Cahill, Thomas M

    2014-08-19

    Synchrotron radiation X-ray fluorescence (SR-XRF) is a powerful elemental analysis tool, yet synchrotrons are large, multiuser facilities that are generally not amenable to modification. However, the X-ray beamlines from synchrotrons can be modified by simply including X-ray filters or removing monochromators to improve the SR-XRF analysis. In this study, we evaluated four easily applied beamline configurations for the analysis of three representative environmental samples, namely a thin aerosol sample, an intermediate thickness biological sample, and a thick rare earth mineral specimen. The results showed that the "white beam" configuration, which was simply the full, polychromatic output of the synchrotron, was the optimal configuration for the analysis of thin samples with little mass. The "filtered white beam" configuration removed the lower energy X-rays from the excitation beam so it gave better sensitivity for elements emitting more energetic X-rays. The "filtered white beam-filtered detector" configuration sacrifices the lower energy part of the spectrum (<15 keV) for improved sensitivity in the higher end (∼26 to 48 keV range). The use of a monochromatic beam, which tends to be the standard mode of operation for most SR-XRF analyses reported in the literature, gave the least sensitive analysis.

  2. Atomic structure of machined semiconducting chips: An x-ray absorption spectroscopy study

    SciTech Connect

    Paesler, M.; Sayers, D.

    1988-12-01

    X-ray absorption spectroscopy (XAS) has been used to examine the atomic structure of chips of germanium that were produced by single point diamond machining. It is demonstrated that although the local (nearest neighbor) atomic structure is experimentally quite similar to that of single crystal specimens information from more distant atoms indicates the presence of considerable stress. An outline of the technique is given and the strength of XAS in studying the machining process is demonstrated.

  3. Diagnostic copper imaging of Menkes disease by synchrotron radiation-generated X-ray fluorescence analysis

    PubMed Central

    Kinebuchi, Miyuki; Matsuura, Akihiro; Kiyono, Tohru; Nomura, Yumiko; Kimura, Sachiko

    2016-01-01

    Copper (Cu) is an indispensable metal for normal development and function of humans, especially in central nervous system (CNS). However, its redox activity requires accurate Cu transport system. ATP7A, a main Cu2+ transporting-ATPase, is necessary to efflux Cu across the plasma membrane and synthesize cuproenzymes. Menkes disease (MD) is caused by mutations in ATP7A gene. Clinically, MD is Cu deficiency syndrome and is treated with Cu-histidine injections soon after definite diagnosis. But outcome of the most remains poor. To estimate the standard therapy, Cu distribution in the treated classic MD patients is analyzed by synchrotron-generated X-ray fluorescence technique (SR-XRF), which identifies and quantifies an individual atom up to at subcellular level of resolution with wide detection area. SR-XRF analysis newly reveals that Cu exists in spinal cord parenchyma and flows out via venous and lymph systems. By systemic analysis, excess Cu is detected in the proximal tubular cells of the kidney, the mucosal epithelial cells of the intestine, and the lymph and venous systems. The current study suggests that the standard therapy supply almost enough Cu for patient tissues. But given Cu passes through the tissues to venous and lymph systems, or accumulate in the cells responsible for Cu absorption. PMID:27629586

  4. Total reflection X-ray fluorescence and energy-dispersive X-ray fluorescence analysis of runoff water and vegetation from abandoned mining of Pb Zn ores

    NASA Astrophysics Data System (ADS)

    Marques, A. F.; Queralt, I.; Carvalho, M. L.; Bordalo, M.

    2003-12-01

    The present work reports on the heavy metal content: Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Cd and Pb in running waters and vegetation around abandoned mining areas. Two species of mosses ( Dicranum sp. and Pleurocarpus sp.) and three different species of wild grass ( Bromus sp., Rumex sp. and Pseudoavena sp.) growing on the surrounding areas of old lead-zinc mines (Aran Valley, Pyrenees, NE Spain) have been analyzed. Both water and vegetation were collected in two different sampling places: (a) near the mine gallery water outlets and (b) on the landfill close to the abandoned mineral concentration factories. For the heavy metal content determination, two different techniques were used: total reflection X-ray fluorescence for water analysis and energy-dispersive X-ray fluorescence for vegetation study. Surface waters around mine outlets exhibit anomalous content of Co, Ni, Zn, Cd. Stream waters running on mining landfills exhibit higher Cu, Zn, Cd and Pb than those of the waters at the mine gallery outlets. The results allow us to assess the extent of the environmental impact of the mining activities on the water quality. The intake of these elements by vegetation was related with the sampling place, reflecting the metal water content and the substrate chemistry. Accumulation of metals in mosses is higher than those exhibited in wild grasses. Furthermore, different levels of accumulation were found in different wild grass. Rumex sp. presented the lowest metal concentrations, while Pseudoavena sp. reported the highest metal content.

  5. Chemical analysis of impurity boron atoms in diamond using soft X-ray emission spectroscopy.

    PubMed

    Muramatsu, Yasuji; Iihara, Junji; Takebe, Toshihiko; Denlinger, Jonathan D

    2008-07-01

    To analyze the local structure and/or chemical states of boron atoms in boron-doped diamond, which can be synthesized by the microwave plasma-assisted chemical vapor deposition method (CVD-B-diamond) and the temperature gradient method at high pressure and high temperature (HPT-B-diamond), we measured the soft X-ray emission spectra in the CK and BK regions of B-diamonds using synchrotron radiation at the Advanced Light Source (ALS). X-ray spectral analyses using the fingerprint method and molecular orbital calculations confirm that boron atoms in CVD-B-diamond substitute for carbon atoms in the diamond lattice to form covalent B-C bonds, while boron atoms in HPT-B-diamond react with the impurity nitrogen atoms to form hexagonal boron nitride. This suggests that the high purity diamond without nitrogen impurities is necessary to synthesize p-type B-diamond semiconductors.

  6. Chemical Analysis of Impurity Boron Atoms in Diamond Using Soft X-ray Emission Spectroscopy

    SciTech Connect

    Muramatsu, Yasuji; Iihara, Junji; Takebe, Toshihiko; Denlinger, Jonathan D.

    2008-03-29

    To analyze the local structure and/or chemical states of boron atoms in boron-doped diamond, which can be synthesized by the microwave plasma-assisted chemical vapor deposition method (CVD-B-diamond) and the temperature gradient method at high pressure and high temperature (HPT-B-diamond), we measured the soft X-ray emission spectra in the CK and BK regions of B-diamonds using synchrotron radiation at the Advanced Light Source (ALS). X-ray spectral analyses using the fingerprint method and molecular orbital calculations confirm that boron atoms in CVD-B-diamond substitute for carbon atoms in the diamond lattice to form covalent B-C bonds, while boron atoms in HPT-B-diamond react with the impurity nitrogen atoms to form hexagonal boron nitride. This suggests that the high purity diamond without nitrogen impurities is necessary to synthesize p-type B-diamond semiconductors.

  7. Atomic processes modeling of X-ray free electron laser produced plasmas using SCFLY code

    NASA Astrophysics Data System (ADS)

    Chung, H.-K.; Cho, B. I.; Ciricosta, O.; Vinko, S. M.; Wark, J. S.; Lee, R. W.

    2017-03-01

    With the development of X-ray free electron lasers (XFEL), a novel state of matter of highly transient and non-equilibrium plasma has been created in laboratories. As high intensity X-ray laser beams interact with a solid density target, electrons are ionized from inner-shell orbitals and these electrons and XFEL photons create dense and finite temperature plasmas. In order to study atomic processes in XFEL driven plasmas, the atomic kinetics model SCFLY containing an extensive set of configurations needed for solid density plasmas was applied to study atomic processes of XFEL driven systems. The code accepts the time-dependent conditions of the XFEL as input parameters, and computes time-dependent population distributions and ionization distributions self-consistently with electron temperatures and densities assuming an instantaneous equilibration of electron energies. The methods and assumptions in the atomic kinetics model and unique aspects of atomic processes in XFEL driven plasmas are described.

  8. Characterization of energy response for photon-counting detectors using x-ray fluorescence

    PubMed Central

    Ding, Huanjun; Cho, Hyo-Min; Barber, William C.; Iwanczyk, Jan S.; Molloi, Sabee

    2014-01-01

    Purpose: To investigate the feasibility of characterizing a Si strip photon-counting detector using x-ray fluorescence. Methods: X-ray fluorescence was generated by using a pencil beam from a tungsten anode x-ray tube with 2 mm Al filtration. Spectra were acquired at 90° from the primary beam direction with an energy-resolved photon-counting detector based on an edge illuminated Si strip detector. The distances from the source to target and the target to detector were approximately 19 and 11 cm, respectively. Four different materials, containing silver (Ag), iodine (I), barium (Ba), and gadolinium (Gd), were placed in small plastic containers with a diameter of approximately 0.7 cm for x-ray fluorescence measurements. Linear regression analysis was performed to derive the gain and offset values for the correlation between the measured fluorescence peak center and the known fluorescence energies. The energy resolutions and charge-sharing fractions were also obtained from analytical fittings of the recorded fluorescence spectra. An analytical model, which employed four parameters that can be determined from the fluorescence calibration, was used to estimate the detector response function. Results: Strong fluorescence signals of all four target materials were recorded with the investigated geometry for the Si strip detector. The average gain and offset of all pixels for detector energy calibration were determined to be 6.95 mV/keV and −66.33 mV, respectively. The detector’s energy resolution remained at approximately 2.7 keV for low energies, and increased slightly at 45 keV. The average charge-sharing fraction was estimated to be 36% within the investigated energy range of 20–45 keV. The simulated detector output based on the proposed response function agreed well with the experimental measurement. Conclusions: The performance of a spectral imaging system using energy-resolved photon-counting detectors is very dependent on the energy calibration of the

  9. Optimizing detector geometry for trace element mapping by X-ray fluorescence

    SciTech Connect

    Sun, Yue; Gleber, Sophie -Charlotte; Jacobsen, Chris; Kirz, Janos; Vogt, Stefan

    2015-01-01

    We report that trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. In conclusion, we conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.

  10. Optimizing detector geometry for trace element mapping by X-ray fluorescence

    PubMed Central

    Sun, Yue; Gleber, Sophie-Charlotte; Jacobsen, Chris; Kirz, Janos; Vogt, Stefan

    2016-01-01

    Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples. PMID:25600825

  11. Optimizing detector geometry for trace element mapping by X-ray fluorescence

    DOE PAGES

    Sun, Yue; Gleber, Sophie -Charlotte; Jacobsen, Chris; ...

    2015-01-01

    We report that trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral responsemore » of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. In conclusion, we conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.« less

  12. Optimizing detector geometry for trace element mapping by X-ray fluorescence.

    PubMed

    Sun, Yue; Gleber, Sophie-Charlotte; Jacobsen, Chris; Kirz, Janos; Vogt, Stefan

    2015-05-01

    Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples.

  13. Combined X-ray fluorescence and absorption computed tomography using a synchrotron beam

    NASA Astrophysics Data System (ADS)

    Hall, C.

    2013-06-01

    X-ray computed tomography (CT) and fluorescence X-ray computed tomography (FXCT) using synchrotron sources are both useful tools in biomedical imaging research. Synchrotron CT (SRCT) in its various forms is considered an important technique for biomedical imaging since the phase coherence of SR beams can be exploited to obtain images with high contrast resolution. Using a synchrotron as the source for FXCT ensures a fluorescence signal that is optimally detectable by exploiting the beam monochromaticity and polarisation. The ability to combine these techniques so that SRCT and FXCT images are collected simultaneously, would bring distinct benefits to certain biomedical experiments. Simultaneous image acquisition would alleviate some of the registration difficulties which comes from collecting separate data, and it would provide increased information about the sample: functional X-ray images from the FXCT, with the morphological information from the SRCT. A method is presented for generating simultaneous SRCT and FXCT images. Proof of principle modelling has been used to show that it is possible to recover a fluorescence image of a point-like source from an SRCT apparatus by suitably modulating the illuminating planar X-ray beam. The projection image can be successfully used for reconstruction by removing the static modulation from the sinogram in the normal flat and dark field processing. Detection of the modulated fluorescence signal using an energy resolving detector allows the position of a fluorescent marker to be obtained using inverse reconstruction techniques. A discussion is made of particular reconstruction methods which might be applied by utilising both the CT and FXCT data.

  14. Bent Laue X-ray Fluorescence Imaging of Manganese in Biological Tissues--Preliminary Results

    SciTech Connect

    Zhu Ying; Zhang Honglin; Bewer, Brian; Nichol, Helen; Chapman, Dean; Thomlinson, Bill

    2010-06-23

    Manganese (Mn) is not abundant in human brain tissue, but it is recognized as a neurotoxin. The symptoms of manganese intoxication are similar to Parkinson's disease (PD), but the link between environmental, occupational or dietary Mn exposure and PD in humans is not well established. X-ray Absorption Spectroscopy (XAS) and in particular X-ray fluorescence can provide precise information on the distribution, concentration and chemical form of metals. However the scattered radiation and fluorescence from the adjacent abundant element, iron (Fe), may interfere with and limit the ability to detect ultra-dilute Mn. A bent Laue analyzer based Mn fluorescence detection system has been designed and fabricated to improve elemental specificity in XAS imaging. This bent Laue analyzer of logarithmic spiral shape placed upstream of an energy discriminating detector should improve the energy resolution from hundreds of eV to several eV. The bent Laue detection system was validated by imaging Mn fluorescence from Mn foils, gelatin calibration samples and adult Drosophila at the Hard X-ray MicroAnalysis (HXMA) beamline at the Canadian Light Source (CLS). Optimization of the design parameters, fabrication procedures and preliminary experimental results are presented along with future plans.

  15. Bent Laue X-ray Fluorescence Imaging of Manganese in Biological Tissues—Preliminary Results

    NASA Astrophysics Data System (ADS)

    Zhu, Ying; Bewer, Brian; Zhang, Honglin; Nichol, Helen; Thomlinson, Bill; Chapman, Dean

    2010-06-01

    Manganese (Mn) is not abundant in human brain tissue, but it is recognized as a neurotoxin. The symptoms of manganese intoxication are similar to Parkinson's disease (PD), but the link between environmental, occupational or dietary Mn exposure and PD in humans is not well established. X-ray Absorption Spectroscopy (XAS) and in particular X-ray fluorescence can provide precise information on the distribution, concentration and chemical form of metals. However the scattered radiation and fluorescence from the adjacent abundant element, iron (Fe), may interfere with and limit the ability to detect ultra-dilute Mn. A bent Laue analyzer based Mn fluorescence detection system has been designed and fabricated to improve elemental specificity in XAS imaging. This bent Laue analyzer of logarithmic spiral shape placed upstream of an energy discriminating detector should improve the energy resolution from hundreds of eV to several eV. The bent Laue detection system was validated by imaging Mn fluorescence from Mn foils, gelatin calibration samples and adult Drosophila at the Hard X-ray MicroAnalysis (HXMA) beamline at the Canadian Light Source (CLS). Optimization of the design parameters, fabrication procedures and preliminary experimental results are presented along with future plans.

  16. X-ray fluorescence computed tomography (XFCT) imaging of gold nanoparticle-loaded objects using 110 kVp x-rays.

    PubMed

    Cheong, Seong-Kyun; Jones, Bernard L; Siddiqi, Arsalan K; Liu, Fang; Manohar, Nivedh; Cho, Sang Hyun

    2010-02-07

    A conventional x-ray fluorescence computed tomography (XFCT) technique requires monochromatic synchrotron x-rays to simultaneously determine the spatial distribution and concentration of various elements such as metals in a sample. However, the synchrotron-based XFCT technique appears to be unsuitable for in vivo imaging under a typical laboratory setting. In this study we demonstrated, for the first time to our knowledge, the possibility of performing XFCT imaging of a small animal-sized object containing gold nanoparticles (GNPs) at relatively low concentrations using polychromatic diagnostic energy range x-rays. Specifically, we created a phantom made of polymethyl methacrylate plastic containing two cylindrical columns filled with saline solution at 1 and 2 wt% GNPs, respectively, mimicking tumors/organs within a small animal. XFCT scanning of the phantom was then performed using microfocus 110 kVp x-ray beam and cadmium telluride (CdTe) x-ray detector under a pencil beam geometry after proper filtering of the x-ray beam and collimation of the detector. The reconstructed images clearly identified the locations of the two GNP-filled columns with different contrast levels directly proportional to gold concentration levels. On the other hand, the current pencil-beam implementation of XFCT is not yet practical for routine in vivo imaging tasks with GNPs, especially in terms of scanning time. Nevertheless, with the use of multiple detectors and a limited number of projections, it may still be used to image some objects smaller than the current phantom size. The current investigation suggests several modification strategies of the current XFCT setup, such as the adoption of the quasi-monochromatic cone/fan x-ray beam and XFCT-specific spatial filters or pinhole detector collimators, in order to establish the ultimate feasibility of a bench-top XFCT system for GNP-based preclinical molecular imaging applications.

  17. New developments of X-ray fluorescence imaging techniques in laboratory

    NASA Astrophysics Data System (ADS)

    Tsuji, Kouichi; Matsuno, Tsuyoshi; Takimoto, Yuki; Yamanashi, Masaki; Kometani, Noritsugu; Sasaki, Yuji C.; Hasegawa, Takeshi; Kato, Shuichi; Yamada, Takashi; Shoji, Takashi; Kawahara, Naoki

    2015-11-01

    X-ray fluorescence (XRF) analysis is a well-established analytical technique with a long research history. Many applications have been reported in various fields, such as in the environmental, archeological, biological, and forensic sciences as well as in industry. This is because XRF has a unique advantage of being a nondestructive analytical tool with good precision for quantitative analysis. Recent advances in XRF analysis have been realized by the development of new x-ray optics and x-ray detectors. Advanced x-ray focusing optics enables the making of a micro x-ray beam, leading to micro-XRF analysis and XRF imaging. A confocal micro-XRF technique has been applied for the visualization of elemental distributions inside the samples. This technique was applied for liquid samples and for monitoring chemical reactions such as the metal corrosion of steel samples in the NaCl solutions. In addition, a principal component analysis was applied for reducing the background intensity in XRF spectra obtained during XRF mapping, leading to improved spatial resolution of confocal micro-XRF images. In parallel, the authors have proposed a wavelength dispersive XRF (WD-XRF) imaging spectrometer for a fast elemental imaging. A new two dimensional x-ray detector, the Pilatus detector was applied for WD-XRF imaging. Fast XRF imaging in 1 s or even less was demonstrated for Euro coins and industrial samples. In this review paper, these recent advances in laboratory-based XRF imaging, especially in a laboratory setting, will be introduced.

  18. Characterization of phosphorus in organisms at sub-micron resolution using X-ray fluorescence spectromicroscopy.

    SciTech Connect

    Diaz, J.; Ingall, E; Vogt, S; Paterson, D; DeJonge, M; Rao, C; Brandes, J

    2009-01-01

    X-ray spectromicroscopy (combined X-ray spectroscopy and microscopy) is uniquely capable of determining sub-micron scale elemental content and chemical speciation in minimally-prepared particulate samples. The high spatial resolutions achievable with this technique have enabled the close examination of important microscale processes relevant to the cycling of biogeochemically important elements. Here, we demonstrate the value of X-ray microscopy to environmental and biological research by examining the phosphorus and metal chemistry of complete individual cells from the algal genera Chlamydomonas sp. and Chlorella sp. X-ray analysis revealed that both genera store substantial intracellular phosphorus as distinct, heterogeneously distributed granules whose X-ray fluorescence spectra are consistent with that of polyphosphate. Polyphosphate inclusions ranged in size from 0.3-1.4 {micro}m in diameter and exhibited a nonspecies-specific average phosphorus concentration of 6.87 {+-} 1.86 {micro}g cm{sup -2}, which was significantly higher than the average concentration of phosphorus measured in the total cell, at 3.14 {+-} 0.98 {micro}g cm{sup -2} (95% confidence). Polyphosphate was consistently associated with calcium and iron, exhibiting average P:cation molar ratios of 8.31 {+-} 2.00 and 108 {+-} 34, respectively (95% confidence). In some cells, polyphosphate was also associated with potassium, zinc, manganese, and titanium. Based on our results, X-ray spectromicroscopy can provide high-resolution elemental data on minimally prepared, unsectioned cells that are unattainable through alternative microscopic methods and conventional bulk chemical techniques currently available in many fields of marine chemistry.

  19. Disentangling atomic-layer-specific x-ray absorption spectra by Auger electron diffraction spectroscopy

    NASA Astrophysics Data System (ADS)

    Matsui, Fumihiko; Matsushita, Tomohiro; Kato, Yukako; Hashimoto, Mie; Daimon, Hiroshi

    2009-11-01

    In order to investigate the electronic and magnetic structures of each atomic layer at subsurface, we have proposed a new method, Auger electron diffraction spectroscopy, which is the combination of x-ray absorption spectroscopy (XAS) and Auger electron diffraction (AED) techniques. We have measured a series of Ni LMM AED patterns of the Ni film grown on Cu(001) surface for various thicknesses. Then we deduced a set of atomic-layer-specific AED patterns in a numerical way. Furthermore, we developed an algorithm to disentangle XANES spectra from different atomic layers using these atomic-layer-specific AED patterns. Surface and subsurface core level shift were determined for each atomic layer.

  20. Extending synchrotron-based atomic physics experiments into the hard X-ray region

    SciTech Connect

    LeBrun, T.

    1996-12-31

    The high-brightness, hard x-ray beams available from third-generation synchrotron sources are opening new opportunities to study the deepest inner shells of atoms, an area where little work has been done and phenomena not observed in less tightly bound inner-shells are manifested. In addition scattering processes which are weak at lower energies become important, providing another tool to investigate atomic structure as well as an opportunity to study photon/atom interactions beyond photoabsorption. In this contribution the authors discuss some of the issues related to extending synchrotron-based atomic physics experiments into the hard x-ray region from the physical and the experimental point of view. They close with a discussion of a technique, resonant Raman scattering, that may prove invaluable in determining the spectra of the very highly-excited states resulting from the excitation of deep inner shells.

  1. Analytical characterization of a new mobile X-ray fluorescence and X-ray diffraction instrument combined with a pigment identification case study

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Vekemans, Bart; Verhaeven, Eddy; Tack, Pieter; De Wolf, Robin; Garrevoet, Jan; Vandenabeele, Peter; Vincze, Laszlo

    2015-08-01

    A new, commercially available, mobile system combining X-ray diffraction and X-ray fluorescence has been evaluated which enables both elemental analysis and phase identification simultaneously. The instrument makes use of a copper or molybdenum based miniature X-ray tube and a silicon-Pin diode energy-dispersive detector to count the photons originating from the samples. The X-ray tube and detector are both mounted on an X-ray diffraction protractor in a Bragg-Brentano θ:θ geometry. The mobile instrument is one of the lightest and most compact instruments of its kind (3.5 kg) and it is thus very useful for in situ purposes such as the direct (non-destructive) analysis of cultural heritage objects which need to be analyzed on site without any displacement. The supplied software allows both the operation of the instrument for data collection and in-depth data analysis using the International Centre for Diffraction Data database. This paper focuses on the characterization of the instrument, combined with a case study on pigment identification and an illustrative example for the analysis of lead alloyed printing letters. The results show that this commercially available light-weight instrument is able to identify the main crystalline phases non-destructively, present in a variety of samples, with a high degree of flexibility regarding sample size and position.

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

    NASA Astrophysics Data System (ADS)

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

    2003-12-01

    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.

  3. Development of total uranium analytical method by L x-ray fluorescence

    SciTech Connect

    Dewberry, R.A.

    1996-09-18

    This paper describes development of an L x-ray fluorescence technique to perform total uranium analysis using an internal excitation source which is added directly to the sample. The method has been demonstrated with synthetic U samples in the limited concentration range of 1g/l to 15g/l, and provides the advantages of simplicity, involving no mechanical parts which would normally be found in an external excitation source. Total uranium is determined by counting L x-rays fluoresced by a microCurie level spike of Cd-109 added directly to the sample and without shielding the excitation source from the detector. A method for correction of sample self-absorption is included in the analysis.

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

    NASA Astrophysics Data System (ADS)

    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.

  5. Elemental mapping of biofortified wheat grains using micro X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Ramos, I.; Pataco, I. M.; Mourinho, M. P.; Lidon, F.; Reboredo, F.; Pessoa, M. F.; Carvalho, M. L.; Santos, J. P.; Guerra, M.

    2016-06-01

    Micro X-ray fluorescence has been used to obtain elemental maps of biofortified wheat grains. Two varieties of wheat were used in the study, Triticum aestivum L. and Triticum durum desf. Two treatments, with different nutrient concentration, were applied to the plants during the whole plant growth cycle. From the obtained elemental maps it was possible to extract information regarding the plant's physiological processes under the biofortification procedures. Both macro and micronutrients were mapped, providing useful insight into the posterior food processing mechanisms of this biofortified staple food. We have also shown that these kind of studies can now be performed with laboratory benchtop apparatus, rather than using synchrotron radiation, increasing the overall attractiveness of micro X-ray fluorescence in the study of highly heterogeneous biological samples.

  6. [Measurement and analysis of lead in soil using X-ray fluorescence spectroscopy].

    PubMed

    Zhang, Rong; Zhang, Yu-Jun; Zhang, Wei; Chen, Dong; Yu, Xiao-Ya; Gao, Yan-Wei

    2013-02-01

    The present paper analyzed the characteristics of X-ray fluorescence spectroscopy (XRF) of metal element lead in soil using the NITON XLt793 portable X-ray fluorescence spectra of heavy metal analyzer under laboratory conditions. The characteristic spectral lines of L(alpha) (energy: 10. 55 keV) and L(beta) (energy: 12. 61 keV) with different matrix elements were selected respectively for lead in the experiment. By measuring the intensities of the characteristic spectral line with different Pb concentration, the results demonstrate that the relation between concentration [mass fraction 10 x 10(-6) - 1 800 x 10(-6)] of Pb element and the intensity of the characteristic spectrum is well linear. The calibration curve of Pb was plotted based on the different concentration measurement results, and the limit of detection of 7.89 x 10(-6) was obtained for Pb in soil.

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

    PubMed

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

    2016-05-01

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

  8. Intershell correlations in nonresonant Compton scattering of an X-ray photon by an atom

    SciTech Connect

    Hopersky, A. N. Nadolinsky, A. M.; Ikoeva, K. Kh.; Khoroshavina, O. A.

    2011-11-15

    The role of intershell correlations in nonresonant Compton scattering of an X-ray photon by a free multielectron atom is studied theoretically for the Ar atom. The results of calculation are of a predictive nature. The developed mathematical formalism is general in nature and can be applied to a wide set of elements from the Periodic Table, for which the description of the wavefunctions of scattering states in the nonrelativistic Hartree-Fock approximation remains correct.

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

    PubMed Central

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

    2016-01-01

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

  10. Atomic data for the ITER Core Imaging X-ray Spectrometer

    SciTech Connect

    Clementson, J; Beiersdorfer, P; Biedermann, C; Bitter, M; Delgado-Aparicio, L F; Graf, A; Gu, M F; Hill, K W; Barnsley, R

    2012-06-15

    The parameters of the ITER core plasmas will be measured using the Core Imaging X-ray Spectrometer (CIXS), a high-resolution crystal spectrometer focusing on the L-shell spectra of highly ionized tungsten atoms. In order to correctly infer the plasma properties accurate atomic data are required. Here, some aspects of the underlying physics are discussed using experimental data and theoretical predictions from modeling.

  11. Evaluation of Portable X-Ray Fluorescence (XRF) Analyzer for Zirconium-Thickness Measurements

    SciTech Connect

    Glenn Moore

    2013-09-01

    This Technical Evaluation Report provides details of preliminary testing/experiments performed using a handheld X-ray fluorescence analyzer. The analyzer will be utilized in upcoming fuel-foil-rolling optimization studies at the INL. The studies are being performed in support of DOE’s Office of Global Threat Reduction -- Reactor Conversion Subprogram. Details of the equipment used, operating parameters, and measurement results are provided in this report.

  12. Analysis of some Nigerian solid mineral ores by energy-dispersive X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Obiajunwa, E. I.

    2001-11-01

    Determination of major, minor and trace elements in some Nigerian solid mineral ores by energy-dispersive X-ray fluorescence (EDXRF) spectroscopy is described. Concentration values of major, minor and trace elements for Z>18 are reported. The mineral ores studied include (i) tantalite-coloumbite minerals, (ii) bismuth minerals and (iii) lead minerals. The accuracy and precision of the technique for chemical analysis was assured by analysing the geological standards mica-Fe (biotite) and NBS 278 (obsidian).

  13. Use of MCNP code in energy dispersive X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Trojek, T.; Čechák, T.

    2007-10-01

    Monte Carlo simulations enable us to improve the applicability of analytical techniques based on emission of characteristic radiation. In particular, the MCNP4C2 code was tested for interpretation of measured data obtained with the use of energy dispersive X-ray fluorescence analysis. This paper describes MCNP outputs and compares them with the results of analytical calculations or experiments. Then the application of Monte Carlo simulations to the prediction of measurement results is shown, and the MCNP results are verified.

  14. Application of an X-ray Fluorescence Instrument to Helicopter Wear Debris Analysis

    DTIC Science & Technology

    2008-04-01

    Application of an X-ray Fluorescence Instrument to Helicopter Wear Debris Analysis Andrew Becker Air Vehicles Division...instrument to determine the composition of wear debris collected from helicopter magnetic chip detectors and oil filters. The Twin-X XRF (assessed in this...report) is a commercially produced bench-top XRF and has not previously been applied to wear debris analysis of Australian Defence Force aircraft

  15. Noninvasive determination of glomerular filtration rate using x-ray fluorescence.

    PubMed

    Alazraki, N; Verba, J W; Henry, J E; Becker, R; Taylor, A; Halpern, S E

    1977-01-01

    Accurate glomerular filtration rates (GFR) can be calculated based on the infusion of small amounts of nonradioactive iothalamate and collection of plasma samples for assay by x-ray fluorescence. This innovation permits frequent clearance determinations in patients without the hazard of repeated radiation exposure and without the necessity of catheterization of the bladder for urine samples. Thus, the technique becomes feasible in children, transplant patients, and other needing accurate and frequent GFR determinations.

  16. Detection and quantification of trace elements in rice and rice products using x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Foran, Kelly A.; Fleming, David E. B.

    2015-12-01

    We used X-ray fluorescence (XRF) to examine the presence of arsenic (As) and other trace elements (manganese, iron, nickel, copper, and zinc) in rice and rice products. A portable XRF analyzer was used to test samples, and amplitudes for the analyzed elements were identified in the resulting data. The detection limit of the system was sufficiently low to detect As in some rice and rice product samples.

  17. X-ray fluorescence analysis of metal concentration in an alloy electroplating bath

    SciTech Connect

    Hines, R.A.

    1980-06-01

    An energy-dispersive x-ray fluorescence analysis system has been developed for rapid, simultaneous analysis of gold and copper concentrations in an aqueous electroplating bath. The speed and repeatability of the system make it well suited for in-process control. Data collection and reduction are automatic. The analysis requires less than 10 minutes from taking the sample to printing the gold and copper concentrations.

  18. X-Ray Fluorescence Holographic Study on a Single-Crystal Thin Film of a Rewritable Optical Media

    SciTech Connect

    Hosokawa, S.; Ozaki, T.; Hayashi, K.; Happo, N.; Horii, K.; Fons, P.; Tominaga, J.; Kolobov, A. V.

    2007-01-19

    In this article, we discuss X-ray fluorescence holography (XFH) using a third-generation synchrotron radiation facility through an application to a DVD-RAM material thin film. Three-dimensional atomic images were obtained at 100 K around the Ge atoms in a Ge2Sb2Te5 single-crystal thin film by means of XFH technique at the beamline BL37XU of the SPring-8 to clarify the high-speed writing and erasing mechanism of this DVD material. From the obtained XFH images, it was concluded that the single-crystal thin film has a mixture of rocksalt and zinc-blende structures. In addition, the images indicate large distortions associated with the existence of vacancies of the Ge(Sb) site. The present XFH results are in good agreement with the previous XAFS results, which has predicted a phase transition due to an umbrella flip motion of the Ge atom000.

  19. A method of measuring gold nanoparticle concentrations by x-ray fluorescence for biomedical applications

    SciTech Connect

    Wu Di; Li Yuhua; Wong, Molly D.; Liu Hong

    2013-05-15

    Purpose: This paper reports a technique that enables the quantitative determination of the concentration of gold nanoparticles (GNPs) through the accurate detection of their fluorescence radiation in the diagnostic x-ray spectrum. Methods: Experimentally, x-ray fluorescence spectra of 1.9 and 15 nm GNP solutions are measured using an x-ray spectrometer, individually and within chicken breast tissue samples. An optimal combination of excitation and emission filters is determined to segregate the fluorescence spectra at 66.99 and 68.80 keV from the background scattering. A roadmap method is developed that subtracts the scattered radiation (acquired before the insertion of GNP solutions) from the signal radiation acquired after the GNP solutions are inserted. Results: The methods effectively minimize the background scattering in the spectrum measurements, showing linear relationships between GNP solutions from 0.1% to 10% weight concentration and from 0.1% to 1.0% weight concentration inside a chicken breast tissue sample. Conclusions: The investigation demonstrated the potential of imaging gold nanoparticles quantitatively in vivo for in-tissue studies, but future studies will be needed to investigate the ability to apply this method to clinical applications.

  20. A New Workflow for x-ray fluorescence tomography: MAPSToTomoPy

    PubMed Central

    Hong, Young Pyo; Chen, Si; Jacobsen, Chris

    2016-01-01

    X-ray fluorescence tomography involves the acquisition of a series of 2D x-ray fluorescence datasets between which a specimen is rotated. At the Advanced Photon Source at Argonne National Laboratory, the workflow at beamlines 2-ID-E and 21-ID-D (the Bionanoprobe, a cryogenic microscope system) has included the use of the program MAPS for obtaining elemental concentrations from 2D images, and the program TomoPy which was developed to include several tomographic reconstruction methods for x-ray transmission data. In the past, fluorescence projection images from an individual chemical element were hand-assembled into a 3D dataset for reconstruction using interactive tools such as ImageJ. We describe here the program MAPSToTomoPy, which provides a graphical user interface (GUI) to control a workflow between MAPS and TomoPy, with tools for visualizing the sinograms of projection image sequences from particular elements and to use these to help correct misalignments of the rotation axis. The program also provides an integrated output of the 3D distribution of the detected elements for subsequent 3D visualization packages. PMID:27103755

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

    PubMed

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

    2015-07-01

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

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

    PubMed Central

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

    2015-01-01

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

  3. The first microbeam synchrotron X-ray fluorescence beamline at the Siam Photon Laboratory.

    PubMed

    Tancharakorn, Somchai; Tanthanuch, Waraporn; Kamonsutthipaijit, Nuntaporn; Wongprachanukul, Narupon; Sophon, Methee; Chaichuay, Sarunyu; Uthaisar, Chunmanus; Yimnirun, Rattikorn

    2012-07-01

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

  4. Portable apparatus for in situ x-ray diffraction and fluorescence analyses of artworks.

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques.

  5. Radiotherapy for cancer using X-ray fluorescence emitted from iodine

    PubMed Central

    Tamura, Masato; Ito, Hiromu; Matsui, Hirofumi

    2017-01-01

    Radiation treatment is popular and the apparatus is already available in many hospitals. Conventional radiation treatment by itself is not sufficient to achieve complete cure. Therefore, radiosensitizers have been developed to enhance the therapeutic effects of the treatment. The concept of radiosensitization with high-Z-elements was first considered many decades ago. However, radiosensitizers are not commonly used in the clinical setting. Here, we propose a radiotherapy method that utilizes fluorescent X-ray emissions from iodine. This approach should achieve a greater therapeutic effect than that of conventional radiotherapy treatments. In our radiotherapy, iomeprol was used as the iodine-donor. The X-ray apparatus with copper and aluminum filters could be used for the X-ray irradiation, the apparatus is not needed for exclusive use. The X-ray apparatus is only required to prepare the copper and aluminum filters. As proof-of-concept, we show that tumor growth was attenuated using this treatment with iomeprol. PMID:28252657

  6. LabVIEW control software for scanning micro-beam X-ray fluorescence spectrometer.

    PubMed

    Wrobel, Pawel; Czyzycki, Mateusz; Furman, Leszek; Kolasinski, Krzysztof; Lankosz, Marek; Mrenca, Alina; Samek, Lucyna; Wegrzynek, Dariusz

    2012-05-15

    Confocal micro-beam X-ray fluorescence microscope was constructed. The system was assembled from commercially available components - a low power X-ray tube source, polycapillary X-ray optics and silicon drift detector - controlled by an in-house developed LabVIEW software. A video camera coupled to optical microscope was utilized to display the area excited by X-ray beam. The camera image calibration and scan area definition software were also based entirely on LabVIEW code. Presently, the main area of application of the newly constructed spectrometer is 2-dimensional mapping of element distribution in environmental, biological and geological samples with micrometer spatial resolution. The hardware and the developed software can already handle volumetric 3-D confocal scans. In this work, a front panel graphical user interface as well as communication protocols between hardware components were described. Two applications of the spectrometer, to homogeneity testing of titanium layers and to imaging of various types of grains in air particulate matter collected on membrane filters, were presented.

  7. X-ray optics for scanning fluorescence microscopy and other applications

    SciTech Connect

    Ryon, R.W.; Warburton, W.K.

    1992-05-01

    Scanning x-ray fluorescence microscopy is analogous to scanning electron microscopy. Maps of chemical element distribution are produced by scanning with a very small x-ray beam. Goal is to perform such scanning microscopy with resolution in the range of <1 to 10 {mu}m, using standard laboratory x-ray tubes. We are investigating mirror optics in the Kirkpatrick-Baez (K-B) configuration. K-B optics uses two curved mirrors mounted orthogonally along the optical axis. The first mirror provides vertical focus, the second mirror provides horizontal focus. We have used two types of mirrors: synthetic multilayers and crystals. Multilayer mirrors are used with lower energy radiation such as Cu K{alpha}. At higher energies such as Ag K{alpha}, silicon wafers are used in order to increase the incidence angles and thereby the photon collection efficiency. In order to increase the surface area of multilayers which reflects x-rays at the Bragg angle, we have designed mirrors with the spacing between layers graded along the optic axis in order to compensate for the changing angle of incidence. Likewise, to achieve a large reflecting surface with silicon, the wafers are placed on a specially designed lever arm which is bent into a log spiral by applying force at one end. In this way, the same diffracting angle is maintained over the entire surface of the wafer, providing a large solid angle for photon collection.

  8. X-ray fluorescence analysis of cultural artefacts — Applications to the Czech heritage

    NASA Astrophysics Data System (ADS)

    Trojek, T.; Musílek, L.; Čechák, T.

    2014-02-01

    X-ray florescence analysis is an excellent non-destructive tool for analysing the elemental composition of materials in a wide range of works of art. The Department of Dosimetry and Application of Ionising Radiation at CTU-FNSPE has used radionuclide or X-ray tube excited energy dispersive X-ray fluorescence for many kinds of artefacts, including frescos, paintings, manuscripts, metal sculptures and other objects, ceramics, jewellery, various archaeological finds, etc. The method used is more or less "traditional", i.e., semiconductor spectrometry of excited X-rays, with some optional choices—capillary optics for collimation of exciting beams and two-dimensional scanning. The "hardware" complex is supplemented by techniques for estimating the depth distribution of measured elements, for suppressing surface effects, for in situ non-contact measurements, etc. Extending the measurable range to lighter elements and decreasing the detection limits is one of the achievements that has been attained by improving the instrumentation and techniques that are used. This paper gives a brief review of works carried out at the Department of Dosimetry and Application of Ionising Radiation at CTU-FNSPE.

  9. Handheld X-ray Fluorescence Spectrometers: Radiation Exposure Risks of Matrix-Specific Measurement Scenarios.

    PubMed

    Rouillon, Marek; Kristensen, Louise J; Gore, Damian B

    2015-07-01

    This study investigates X-ray intensity and dispersion around handheld X-ray fluorescence (XRF) instruments during the measurement of a range of sample matrices to establish radiation exposure risk during operation. Four handheld XRF instruments representing three manufacturers were used on four smooth, flat-lying materials of contrasting matrix composition. Dose rates were measured at 10, 20, 30, and 40 cm intervals every 30° around the instrument at 0 and 45° from the horizontal, as well as vertically from the instrument screen. The analysis of polyethylene recorded dose rates 156 times higher (on average) than steel measurements and 34 times higher than both quartz sand and quartz sandstone. A worst-case exposure scenario was assumed where a user analyses a polyethylene material at arms reach for 1 h each working day for one year. This scenario resulted in an effective body dose of 73.5 μSv, equivalent to three to four chest X-rays (20 μSv) a year, 20 times lower than the average annual background radiation exposure in Australia and well below the annual exposure limit of 1 mSv for non-radiation workers. This study finds the advantages of using handheld XRF spectrometers far outweighs the risk of low radiation exposure linked to X-ray scattering from samples.

  10. Validation of the Geant4 Monte Carlo package for X-ray fluorescence spectroscopy in triaxial geometry

    NASA Astrophysics Data System (ADS)

    Amaro, Pedro; Santos, José Paulo; Samouco, Ana; Adão, Ricardo; Martins, Luís Souto; Weber, Sebastian; Tashenov, Stanislav; Carvalho, Maria Luisa; Pessanha, Sofia

    2017-04-01

    In this study, we investigated the potential of the Geant4 Monte Carlo simulation package for retrieving accurate elemental concentrations from energy dispersive X-ray fluorescence spectra. For this purpose, we implemented a Geant4 code that simulates an energy dispersive X-ray fluorescence spectrometer in a triaxial geometry. In parallel, we also performed measurements in a spectrometer with the same geometry, for validation of the present code. This spectrometer allows low limits of detection and permits an effective comparison of elemental concentrations down to tens of part-per-million. Several standard reference materials of both light, medium and heavy matrices were employed in order to attest the validity of simulations for several values of averaged atomic number. We observed good agreement of better than 25% for most fluorescence lines of interest, and for all materials. Discrepancies were observed at the multiple Compton scattering tail. We thus concluded from this experimental and theoretical study that the present Geant4 code can be incorporated in a quantitative method for the determination of trace elements in a triaxial-type spectrometer.

  11. Atomic Data Needs for the New Generation of X-ray Observatories

    NASA Astrophysics Data System (ADS)

    Garcia, Javier; 6174967980

    2016-06-01

    Modeling X-ray spectra produced by photoionized plasmas is crucial for the physical interpretation of many astrophysical sources. These models rely on theoretical and numerical techniques, but importantly also on the availability of reliable atomic data. The need for accurate data continues to grow with the advent of new and more sensitive instruments. I will describe atomic-data requirements for addressing three astrophysical problems: (1) atomic, molecular, and dust absorption in the ISM; (2) detection and characterization of inner-shell lines from various trace elements or Fe-peak elements (e.g., P, K, Cr, Mn, Co); and (3) modeling X-ray spectra reflected from black hole accretion disks in the high-density limit. I will discuss the importance ofthese studies, and the limitations of the theoretical models presently being used to fit data from such current missions as NuSTAR and Astro-H (Hitomi).

  12. Theory of x-ray absorption by laser-dressed atoms

    NASA Astrophysics Data System (ADS)

    Buth, Christian; Santra, Robin

    2007-03-01

    An ab initio theory is devised for the x-ray photoabsorption cross section of atoms in the field of a moderately intense optical laser ( 800nm , 1013W/cm2 ). The laser dresses the core-excited atomic states, which introduces a dependence of the cross section on the angle between the polarization vectors of the two linearly polarized radiation sources. We use the Hartree-Fock-Slater approximation to describe the atomic many-particle problem in conjunction with a nonrelativistic quantum-electrodynamic approach to treat the photon-electron interaction. The continuum wave functions of ejected electrons are treated with a complex absorbing potential that is derived from smooth exterior complex scaling. The solution to the two-color (x-ray plus laser) problem is discussed in terms of a direct diagonalization of the complex symmetric matrix representation of the Hamiltonian. Alternative treatments with time-independent and time-dependent non-Hermitian perturbation theories are presented that exploit the weak interaction strength between x rays and atoms. We apply the theory to study the photoabsorption cross section of krypton atoms near the K edge. A pronounced modification of the cross section is found in the presence of the optical laser.

  13. Assessment of asthmatic inflammation using hybrid fluorescence molecular tomography-x-ray computed tomography

    NASA Astrophysics Data System (ADS)

    Ma, Xiaopeng; Prakash, Jaya; Ruscitti, Francesca; Glasl, Sarah; Stellari, Fabio Franco; Villetti, Gino; Ntziachristos, Vasilis

    2016-01-01

    Nuclear imaging plays a critical role in asthma research but is limited in its readings of biology due to the short-lived signals of radio-isotopes. We employed hybrid fluorescence molecular tomography (FMT) and x-ray computed tomography (XCT) for the assessment of asthmatic inflammation based on resolving cathepsin activity and matrix metalloproteinase activity in dust mite, ragweed, and Aspergillus species-challenged mice. The reconstructed multimodal fluorescence distribution showed good correspondence with ex vivo cryosection images and histological images, confirming FMT-XCT as an interesting alternative for asthma research.

  14. Monochromatic X-ray propagation in multi-Z media for imaging and diagnostics including Kα Resonance Fluorescence

    NASA Astrophysics Data System (ADS)

    Westphal, Maximillian; Lim, Sara; Nahar, Sultana; Pradhan, Anil

    2016-05-01

    Aimed at monochromatic X-ray imaging and therapy, broadband, monochromatic, and quasi-monochromatic X-ray sources and propagation through low and high-Z (HZ) media were studied with numerically and experimentally. Monte Carlo simulations were performed using the software package Geant4, and a new code Photx, to simulate X-ray image contrast, depth of penetration, and total attenuation. The data show that monochromatic and quasi-monochromatic X-rays achieve improved contrast at lower absorbed radiation doses compared to conventional broadband 120 kV or CT scans. Experimental quasi-monochromatic high-intensity laser-produced plasma sources and monochromatic synchrotron beam data are compared. Physical processes responsible for X-ray photoexcitation and absorption are numerically modelled, including a novel mechanism for accelerating Kα resonance fluorescence via twin monochromatic X-ray beam. Potential applications are medical diagnostics and high-Z material detection. Acknowledgement: Ohio Supercomputer Center, Columbus, OH.

  15. A new method for x-ray fluorescence analysis of contaminated material. Final Report

    SciTech Connect

    Grodzins, Lee; Niland, John

    2002-05-23

    Niton has successfully completed the objectives of the Phase II program to build a hand-held, x-ray fluorescent analyzer optimized for DOE decontamination and decommissioning activities in the field. A two-pound x-ray fluorescence analyzer was developed that contains 3 radioactive sources, emitting 3 widely spaced monochromatic x-rays, to give the lowest detection limits for the full range of toxic elements, from chromium to plutonium. A rapid, fundamental- parameters algorithm was developed that yields quantitative results in less than 1 second. High-resolution silicon drift detectors and silicon PIN diodes give excellent efficiency and speed. These results from Phase II have been introduced into the XL 300, 700 and 800 commercial products series. More than 800 of these instruments, yielding revenues of more than $20 million dollars, have been sold since the first 3-source instrument was introduced in 1998. A direct consequence of the Phase II funding has been the growth of Niton from 20 people to its present size of 60.

  16. A novel portable energy dispersive X-ray fluorescence spectrometer with triaxial geometry

    NASA Astrophysics Data System (ADS)

    Pessanha, S.; Alves, M.; Sampaio, J. M.; Santos, J. P.; Carvalho, M. L.; Guerra, M.

    2017-01-01

    The X-ray fluorescence technique is a powerful analytical tool with a broad range of applications such as quality control, environmental contamination by heavy metals, cultural heritage, among others. For the first time, a portable energy dispersive X-ray fluorescence spectrometer was assembled, with orthogonal triaxial geometry between the X-ray tube, the secondary target, the sample and the detector. This geometry reduces the background of the measured spectra by reducing significantly the Bremsstrahlung produced in the tube through polarization in the secondary target and in the sample. Consequently, a practically monochromatic excitation energy is obtained. In this way, a better peak-background ratio is obtained compared to similar devices, improving the detection limits and leading to superior sensitivity. The performance of this setup is compared with the one of a benchtop setup with triaxial geometry and a portable setup with planar geometry. Two case studies are presented concerning the analysis of a 18th century paper document, and the bone remains of an individual buried in the early 19th century.

  17. Development of a single-cell X-ray fluorescence flow cytometer

    SciTech Connect

    Crawford, Andrew M.; Kurecka, Patrick; Yim, Tsz Kwan; Kozemchak, Claire; Deb, Aniruddha; Dostal, Lubomir; Sun, Cheng -Jun; Brewe, Dale L.; Barrea, Raul; Penner-Hahn, James E.

    2016-06-17

    An X-ray fluorescence flow cytometer that can determine the total metal content of single cells has been developed. Capillary action or pressure was used to load cells into hydrophilic or hydrophobic capillaries, respectively. Once loaded, the cells were transported at a fixed vertical velocity past a focused X-ray beam. X-ray fluorescence was then used to determine the mass of metal in each cell. By making single-cell measurements, the population heterogeneity for metals in the µM to mM concentration range on fL sample volumes can be directly measured, a measurement that is difficult using most analytical methods. This approach has been used to determine the metal composition of 936 individual bovine red blood cells (bRBC), 31 individual 3T3 mouse fibroblasts (NIH3T3) and 18 Saccharomyces cerevisiae (yeast) cells with an average measurement frequency of ~4 cells min–1. These data show evidence for surprisingly broad metal distributions. Lastly, details of the device design, data analysis and opportunities for further sensitivity improvement are described.

  18. Development of a single-cell X-ray fluorescence flow cytometer

    DOE PAGES

    Crawford, Andrew M.; Kurecka, Patrick; Yim, Tsz Kwan; ...

    2016-06-17

    An X-ray fluorescence flow cytometer that can determine the total metal content of single cells has been developed. Capillary action or pressure was used to load cells into hydrophilic or hydrophobic capillaries, respectively. Once loaded, the cells were transported at a fixed vertical velocity past a focused X-ray beam. X-ray fluorescence was then used to determine the mass of metal in each cell. By making single-cell measurements, the population heterogeneity for metals in the µM to mM concentration range on fL sample volumes can be directly measured, a measurement that is difficult using most analytical methods. This approach has beenmore » used to determine the metal composition of 936 individual bovine red blood cells (bRBC), 31 individual 3T3 mouse fibroblasts (NIH3T3) and 18 Saccharomyces cerevisiae (yeast) cells with an average measurement frequency of ~4 cells min–1. These data show evidence for surprisingly broad metal distributions. Lastly, details of the device design, data analysis and opportunities for further sensitivity improvement are described.« less

  19. Basic principles of Synchrotron Radiation-Induced X-Ray Fluorescence (SRXRF)

    SciTech Connect

    Gigante, G.E. . Dipt. di Fisica); Hanson, A.L. )

    1990-05-01

    The characteristic x rays can be used as powerful analytical tools for qualitative and quantitative determination of the major, minor and trace composition of materials. X Ray Fluorescence (XRF) techniques used for almost four decade to solve many problems in basic, applied science, and in industry. The XRF techniques that were developed initially used crystal spectrometers, and are referred to in literature as Wavelength Dispersive (WD) techniques. These WD techniques are still used in many fields and have the merit of a excellent energy resolution that allows for the analysis of many elements while avoiding the overlapping of some fluorescence peaks. They are also particularly useful in a matrix that produces copious quantities of a particular radiation. The principal disadvantages of a WD system are the low efficiency of crystal and the reduced energy region in which crystal spectrometer can be used. In the 1960's, Solid State Detectors (SSD) were developed with energy resolution such that the Energy Dispersive XRF techniques could be developed. These SSD's overcame some of the limitations of the WD techniques. The most attractive characteristics of the EDXRF techniques are in their intrinsic multielemental and non destructive capabilities. The development of the high intensity, high brilliance Synchrotron Radiation (SR) sources have open the possibility to make microanalyses using the XRF techniques, increasing the interest of the scientific community for these techniques. In this paper the basic concepts of the XRF technique are reviewed taking in account the availability of the new sources of x rays. 32 refs., 7 figs.

  20. Determination of minor and trace elements in kidney stones by x-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Srivastava, Anjali; Heisinger, Brianne J.; Sinha, Vaibhav; Lee, Hyong-Koo; Liu, Xin; Qu, Mingliang; Duan, Xinhui; Leng, Shuai; McCollough, Cynthia H.

    2014-03-01

    The determination of accurate material composition of a kidney stone is crucial for understanding the formation of the kidney stone as well as for preventive therapeutic strategies. Radiations probing instrumental activation analysis techniques are excellent tools for identification of involved materials present in the kidney stone. In particular, x-ray fluorescence (XRF) can be very useful for the determination of minor and trace materials in the kidney stone. The X-ray fluorescence measurements were performed at the Radiation Measurements and Spectroscopy Laboratory (RMSL) of department of nuclear engineering of Missouri University of Science and Technology and different kidney stones were acquired from the Mayo Clinic, Rochester, Minnesota. Presently, experimental studies in conjunction with analytical techniques were used to determine the exact composition of the kidney stone. A new type of experimental set-up was developed and utilized for XRF analysis of the kidney stone. The correlation of applied radiation source intensity, emission of X-ray spectrum from involving elements and absorption coefficient characteristics were analyzed. To verify the experimental results with analytical calculation, several sets of kidney stones were analyzed using XRF technique. The elements which were identified from this techniques are Silver (Ag), Arsenic (As), Bromine (Br), Chromium (Cr), Copper (Cu), Gallium (Ga), Germanium (Ge), Molybdenum (Mo), Niobium (Nb), Rubidium (Rb), Selenium (Se), Strontium (Sr), Yttrium (Y), Zirconium (Zr). This paper presents a new approach for exact detection of accurate material composition of kidney stone materials using XRF instrumental activation analysis technique.

  1. Quantifying trace elements in individual aquatic protist cells with a synchrotron x-ray fluorescence microprobe.

    SciTech Connect

    Twining, B. S.; Baines, S. B.; Fisher, N. S.; Maser, J.; Vogt, S.; Jacobsen, C.; Tovar-Sanchez, A.; Sanudo-Wihelmy, S. A.; Experimental Facilities Division; Stony Brook Univ.

    2003-01-01

    The study of trace metal cycling by aquatic protists is limited by current analytical techniques. Standard 'bulk' element analysis techniques that rely on physical separations to concentrate cells for analysis cannot separate cells from co-occurring detrital material or other cells of differing taxonomy or trophic function. Here we demonstrate the ability of a synchrotron-based X-ray fluorescence (SXRF) microprobe to quantify the elements Si, Mn, Fe, Ni, and Zn in individual aquatic protist cells. This technique distinguishes between different types of cells in an assemblage and between cells and other particulate matter. Under typical operating conditions, the minimum detection limits are 7.0 x 10{sup -16} mol {mu}m{sup -2} for Si and between 5.0 x 10{sup -20} and 3.9 x 10{sup -19} mol {mu}m{sup -2} for Mn, Fe, Ni, and Zn; this sensitivity is sufficient to detect these elements in cells from even the most pristine waters as demonstrated in phytoplankton cells collected from remote areas of the Southern Ocean. Replicate analyses of single cells produced variations of <5% for Si, Mn, Fe, and Zn and <10% for Ni. Comparative analyses of cultured phytoplankton cells generally show no significant differences in cellular metal concentrations measured with SXRF and standard bulk techniques (spectrophotometry and graphite furnace atomic absorption spectrometry). SXRF also produces two-dimensional maps of element distributions in cells, thereby providing information not available with other analytical approaches. This technique enables the accurate and precise measurement of trace metals in individual aquatic protists collected from natural environments.

  2. Reverse engineering the ancient ceramic technology based on X-ray fluorescence spectromicroscopy

    SciTech Connect

    Sciau, Philippe; Leon, Yoanna; Goudeau, Philippe; Fakra, Sirine C.; Webb, Sam; Mehta, Apurva

    2011-07-06

    We present results of X-ray fluorescence (XRF) microprobe analyses of ancient ceramic cross-sections aiming at deciphering the different firing protocols used for their production. Micro-focused XRF elemental mapping, Fe chemical mapping and Fe K-edge X-ray absorption near edge structure spectroscopy were performed on pre-sigillata ceramics from southern Gaul, and terra Sigillata vessels from Italy and southern Gaul. Pieces from the different workshops and regions showed significant difference in the starting clay material, clay conditioning and kiln firing condition. By contrast, sherds from the same workshop exhibited more subtle differences and possible misfirings. Understanding the precise firing conditions and protocols would allow recreation of kilns for various productions. Furthermore, evolution and modification of kiln design would shed some light on how ancient potters devised solutions to diverse technological problems they encountered.

  3. A hybrid fluorescence tomography and x-ray CT system for quantitative molecular imaging

    NASA Astrophysics Data System (ADS)

    Lin, Yuting; Barber, William C.; Iwanczk, Jan S.; Roeck, Werner W.; Nalcioglu, Orhan; Gulsen, Gultekin

    2010-02-01

    A gantry-based hybrid fluorescence and x-ray computed tomography (FT/CT) system is developed for quantitative molecular imaging. The performance of the dual modality FT/CT system is evaluated using an irregular shaped phantom with an inclusion containing Indocyanine-Green (ICG). The anatomical data from CT provides structural a priori information for the FT inverse problem. Although a 4.2 mm diameter inclusion can be resolved in the reconstructed concentration image without any a priori information, ICG concentration in the inclusion is recovered with 75% error. On the other hand, the error in the recovered ICG concentration reduces to 15% when a priori information from CT is utilized. The results demonstrate that accurate fluorophore concentration can only be obtained when x-ray CT structural a priori information is available.

  4. Elemental investigation on Spanish dinosaur bones by x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Brunetti, Antonio; Piga, Giampaolo; Lasio, Barbara; Golosio, Bruno; Oliva, Piernicola; Stegel, Giovanni; Enzo, Stefano

    2013-07-01

    In this paper we examine the chemical composition results obtained on a collection of 18 dinosaur fossil bones from Spain studied using a portable x-ray fluorescence spectrometer together with a reverse Monte Carlo numerical technique of data analysis. This approach is applied to the hypothesis of arbitrarily rough surfaces in order to account for the influence of the surface state of specimens on the chemical content evaluation. It is confirmed that the chemical content of elements is essential for understanding the changes brought about by diagenetic and taphonomic processes. However, for precise knowledge of what changes fossil bones have undergone after animal life and burial, it is necessary to use a multi-technique approach making use of other instruments like x-ray diffraction in order to describe accurately the transformations undergone by the mineralogical and bioinorganic phases and the properties of specific molecular groups.

  5. ROLE OF X-RAY FLUORESCENCE IN A MODERN GEOCHEMICAL LABORATORY.

    USGS Publications Warehouse

    Taggart, Joseph E.

    1985-01-01

    Because modern geochemical laboratories can seldom have all new analytical equipment, it is clear that priorities must be assigned and choices made when selecting each new instrument. X-ray fluorescence (XRF) spectroscopy has come to play a vital role in this environment largely because it is a dependable, multielement, rapid method that covers a wide range of elemental concentrations, commonly with only one sample preparation. The following discussion centers on the role of modern XRF instrumentation in the resolution of geochemical problems. In order to present a comprehensive view of this role, this paper draws upon a great deal of information from numerous X-ray laboratories visited in the United States and Canada.

  6. Use of x-ray fluorescence and diffraction techniques in studying ancient ceramics of Sri Lanka

    NASA Astrophysics Data System (ADS)

    Karunaratne, B. S. B.

    2012-07-01

    Ceramics were produced for centuries in Sri Lanka for various purposes. Ancient ceramic articles such as pottery, bricks, tiles, sewer pipes, etc, were made from naturally occurring raw materials. Use of X-ray fluorescence (XRF), X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM) in characterizing of two ancient ceramic samples from two different archaeological sites in Sri Lanka is presented. The information obtained in this manner is used to figure out the ancient ceramic technology, particularly to learn about the raw materials used, the source of raw materials, processing parameters such as firing temperature or binders used in ceramic production. This information then can be used to explore the archaeometric background such as the nature and extent of cultural and technological interaction between different periods of history in Sri Lanka.

  7. Experimental demonstration of novel imaging geometries for x-ray fluorescence computed tomography

    PubMed Central

    Fu, Geng; Meng, Ling-Jian; Eng, Peter; Newville, Matt; Vargas, Phillip; Riviere, Patrick La

    2013-01-01

    Purpose: X-ray fluorescence computed tomography (XFCT) is an emerging imaging modality that maps the three-dimensional distribution of elements, generally metals, in ex vivo specimens and potentially in living animals and humans. At present, it is generally performed at synchrotrons, taking advantage of the high flux of monochromatic x rays, but recent work has demonstrated the feasibility of using laboratory-based x-ray tube sources. In this paper, the authors report the development and experimental implementation of two novel imaging geometries for mapping of trace metals in biological samples with ∼50–500 μm spatial resolution. Methods: One of the new imaging approaches involves illuminating and scanning a single slice of the object and imaging each slice's x-ray fluorescent emissions using a position-sensitive detector and a pinhole collimator. The other involves illuminating a single line through the object and imaging the emissions using a position-sensitive detector and a slit collimator. They have implemented both of these using synchrotron radiation at the Advanced Photon Source. Results: The authors show that it is possible to achieve 250 eV energy resolution using an electron multiplying CCD operating in a quasiphoton-counting mode. Doing so allowed them to generate elemental images using both of the novel geometries for imaging of phantoms and, for the second geometry, an osmium-stained zebrafish. Conclusions: The authors have demonstrated the feasibility of these two novel approaches to XFCT imaging. While they use synchrotron radiation in this demonstration, the geometries could readily be translated to laboratory systems based on tube sources. PMID:23718594

  8. Correlative VIS-fluorescence and soft X-ray cryo-microscopy/tomography of adherent cells

    PubMed Central

    Hagen, Christoph; Guttmann, Peter; Klupp, Barbara; Werner, Stephan; Rehbein, Stefan; Mettenleiter, Thomas C.; Schneider, Gerd; Grünewald, Kay

    2012-01-01

    Soft X-ray cryo-microscopy/tomography of vitreous samples is becoming a valuable tool in structural cell biology. Within the ‘water-window’ wavelength region (2.34–4.37 nm), it provides absorption contrast images with high signal to noise ratio and resolution of a few tens of nanometer. Soft X-rays with wavelengths close to the K-absorption edge of oxygen penetrate biological samples with thicknesses in the micrometer range. Here, we report on the application of a recently established extension of the transmission soft X-ray cryo-microscope (HZB TXM) at the beamline U41-XM of the BESSY II electron storage ring by an in-column epi-fluorescence and reflected light cryo-microscope. We demonstrate the new capability for correlative fluorescence and soft X-ray cryo-microscopy/tomography of this instrument along a typical life science experimental approach – the correlation of a fluorophore-tagged protein (pUL34-GFP of pseudorabies virus, PrV, the nuclear membrane-anchored component of the nuclear egress complex of the Herpesviridae which interacts with viral pUL31) in PrV pUL34-GFP/pUL31 coexpressing mammalian cells, with virus-induced vesicular structures in the nucleus, expanding the nucleoplasmic reticulum. Taken together, our results demonstrate new possibilities to study the role of specific proteins in substructures of adherent cells, especially of the nucleus in toto, accessible to electron microscopy in thinned samples only. PMID:22210307

  9. L-shell x-ray fluorescence computed tomography (XFCT) imaging of Cisplatin

    PubMed Central

    Bazalova, Magdalena; Ahmad, Moiz; Pratx, Guillem; Xing, Lei

    2014-01-01

    X-ray fluorescence computed tomography (XFCT) imaging has been focused on the detection of K-shell X-rays. The potential utility of L-shell x-ray XFCT is, however, not well studied. Here we report the first Monte Carlo (MC) simulation of preclinical L-shell XFCT imaging of Cisplatin. We built MC models for both L- and K-shell XFCT with different excitation energies (15 and 30 keV for L-shell and 80 keV for K-shell XFCT). Two small-animal sized imaging phantoms of 2-cm and 4-cm diameter containing a series of objects of 0.6 to 2.7 mm in diameter at 0.7 to 16 mm depths with 10 to 250 μg/mL concentrations of Pt are used in the study. Transmitted and scattered x-rays were collected with photon-integrating transmission detector and photon-counting detector arc, respectively. Collected data were rearranged into XFCT and transmission CT sinograms for image reconstruction. XFCT images were reconstructed with filtered back-projection (FBP) and with iterative maximum-likelihood expectation maximization (ML-EM) without and with attenuation correction. While K-shell XFCT was capable of providing accurate measurement of Cisplatin concentration, its sensitivity was 4.4 and 3.0 times lower than that of L-shell XFCT with 15 keV excitation beam for the 2-cm and 4-cm diameter phantom, respectively. With inclusion of excitation and fluorescence beam attenuation correction, we found that L-shell XFCT was capable of providing fairly accurate information of Cisplatin concentration distribution. With a dose of 29 and 58 mGy, clinically relevant Cisplatin Pt concentrations of 10 μg/mg could be imaged with L-shell XFCT inside a 2-cm and 4-cm diameter object, respectively. PMID:24334507

  10. Rayleigh x-ray scattering from many-electron atoms and ions

    NASA Astrophysics Data System (ADS)

    Surzhykov, A.; Yerokhin, V. A.; Stöhlker, Th; Fritzsche, S.

    2015-07-01

    A theoretical analysis is presented for the elastic Rayleigh scattering of x-rays by many-electron atoms and ions. Special emphasis is placed on the angular distribution and linear polarization of the scattered photons for the case when the incident light is completely (linearly) polarized. Based on second-order perturbation theory and the independent particle approximation, we found that the Rayleigh angular distribution is strongly affected by the charge state and shell structure of the target ions or atoms. This effect can be observed experimentally at modern synchrotron facilities and might provide further insight into the structure of heavy atomic systems.

  11. Advanced combined application of micro-X-ray diffraction/micro-X-ray fluorescence with conventional techniques for the identification of pictorial materials from Baroque Andalusia paintings.

    PubMed

    Herrera, L K; Montalbani, S; Chiavari, G; Cotte, M; Solé, V A; Bueno, J; Duran, A; Justo, A; Perez-Rodriguez, J L

    2009-11-15

    The process of investigating paintings includes the identification of materials to solve technical and historical art questions, to aid in the deduction of the original appearance, and in the establishment of the chemical and physical conditions for adequate restoration and conservation. In particular, we have focused on the identification of several samples taken from six famous canvases painted by Pedro Atanasio Bocanegra, who created a very special collection depicting the life of San Ignacio, which is located in the church of San Justo y Pastor of Granada, Spain. The characterization of the inorganic and organic compounds of the textiles, preparation layers, and pictorial layers have been carried out using an XRD diffractometer, SEM observations, EDX spectrometry, FT-IR spectrometry (both in reflection and transmission mode), pyrolysis/gas chromatography/mass spectrometry and synchrotron-based micro-X-ray techniques. In this work, the advantages over conventional X-ray diffraction of using combined synchrotron-based micro-X-ray diffraction and micro-X-ray fluorescence in the identification of multi-layer paintings is demonstrated.

  12. Direct Determination of Oxidation States of Uranium in Mixed-Valent Uranium Oxides Using Total Reflection X-ray Fluorescence X-ray Absorption Near-Edge Spectroscopy.

    PubMed

    Sanyal, Kaushik; Khooha, Ajay; Das, Gangadhar; Tiwari, M K; Misra, N L

    2017-01-03

    Total reflection X-ray fluorescence (TXRF)-based X-ray absorption near-edge spectroscopy has been used to determine the oxidation state of uranium in mixed-valent U3O8 and U3O7 uranium oxides. The TXRF spectra of the compounds were measured using variable X-ray energies in the vicinity of the U L3 edge in the TXRF excitation mode at the microfocus beamline of the Indus-2 synchrotron facility. The TXRF-based X-ray absorption near-edge spectroscopy (TXRF-XANES) spectra were deduced from the emission spectra measured using the energies below and above the U L3 edge in the XANES region. The data processing using TXRF-XANES spectra of U(IV), U(V), and U(VI) standard compounds revealed that U present in U3O8 is a mixture of U(V) and U(VI), whereas U in U3O7 is mixture of U(IV) and U(VI). The results obtained in this study are similar to that reported in literature using the U M edge. The present study has demonstrated the possibility of application of TXRF for the oxidation state determination and elemental speciation of radioactive substances in a nondestructive manner with very small amount of sample requirement.

  13. Airborne Particulate Matter (PM) filter analysis and modeling by Total reflection X-Ray Fluorescence (TXRF) and X-Ray Standing Wave (XSW)

    PubMed Central

    Borgese, L.; Salmistraro, M.; Gianoncelli, A; Zacco, A.; Lucchini, R.; Zimmerman, N.; Pisani, L.; Siviero, G.; Depero, L. E.; Bontempi, E.

    2011-01-01

    This work is presented as an improvement of a recently introduced method for airborne particulate matter (PM) filter analysis [1]. X-ray Standing Wave (XSW) and Total reflection X-Ray Fluorescence (TXRF) were performed with a new dedicated laboratory instrumentation. The main advantage of performing both XSW and TXRF, is the possibility to distinguish the nature of the sample: if it is a small droplet dry residue, a thin film like or a bulk sample; and to select the angle of total reflection to make TXRF measurements. Finally, the possibility to switch the X-ray source allows to measure with more accuracy lighter and heavier elements (with a a change in X-ray anode, for example from Mo to Cu). The aim of the present study is to lay the theoretical foundation of the new proposed method for airborne PM filters quantitative analysis improving the accuracy and efficiency of quantification by means of an external standard. The theoretical model presented and discussed demonstrated that airborne PM filters can be considered as thin layers. A set of reference samples is prepared in laboratory and used to obtain a calibration curve. Our results demonstrate that the proposed method for quantitative analysis of air PM filters is affordable and reliable without the necessity to digest filters to obtain quantitative chemical analysis, and that the use of XRW improve the accuracy of TXRF analysis. PMID:22284465

  14. Simultaneous measurements of X-ray reflectivity and grazing incidence fluorescence at BL-16 beamline of Indus-2

    SciTech Connect

    Das, Gangadhar; Kane, S. R.; Khooha, Ajay; Singh, A. K.; Tiwari, M. K.

    2015-05-15

    A new multipurpose x-ray reflectometer station has been developed and augmented at the microfocus beamline (BL-16) of Indus-2 synchrotron radiation source to facilitate synchronous measurements of specular x-ray reflectivity and grazing incidence x-ray fluorescence emission from thin layered structures. The design and various salient features of the x-ray reflectometer are discussed. The performance of the reflectometer has been evaluated by analyzing several thin layered structures having different surface interface properties. The results reveal in-depth information for precise determination of surface and interface properties of thin layered materials demonstrating the immense potential of the combined measurements of x-ray reflectivity and grazing incidence fluorescence on a single reflectometer.

  15. Calibration of High-Resolution X-Ray Tomography With Atomic Force Microscopy

    PubMed Central

    Kalukin, Andrew R.; Winn, Barry; Wang, Yuxin; Jacobsen, Chris; Levine, Zachary H.; Fu, Joseph

    2000-01-01

    For two-dimensional x-ray imaging of thin films, the technique of scanning transmission x-ray microscopy (STXM) has achieved images with feature sizes as small as 40 nm in recent years. However, calibration of three-dimensional tomographic images that are produced with STXM data at this scale has not yet been described in the scientific literature, and the calibration procedure has novel problems that have not been encountered by x-ray tomography carried out at a larger scale. In x-ray microtomography, for example, one always has the option of using optical imaging on a section of the object to verify the x-ray projection measurements; with STXM, on the other hand, the sample features are too small to be resolved by light at optical wavelengths. This fact implies that one must rely on procedures with higher resolution, such as atomic force microscopy (AFM), for the calibration. Such procedures, however, generally depend on a highly destructive sectioning of the sample, and are difficult to interpret because they give surface information rather than depth information. In this article, a procedure for calibration is described that overcomes these limitations and achieves a calibration of an STXM tomography image with an AFM image and a scanning electron microscopy image of the same object. A Ge star-shaped pattern was imaged at a synchrotron with a scanning transmission x-ray microscope. Nineteen high-resolution projection images of 200 × 200 pixels were tomographically reconstructed into a three-dimensional image. Features in two-dimensional images as small as 40 nm and features as small as 80 nm in the three-dimensional reconstruction were resolved. Transverse length scales based on atomic force microscopy, scanning electron microscopy, x-ray transmission and tomographic reconstruction agreed to within 10 nm. Toward the center of the sample, the pattern thickness calculated from projection images was (51 ± 15) nm vs (80 ± 52) nm for tomographic reconstruction

  16. Atomic Calculations and Laboratory Measurements Relevant to X-ray Warm Absorbers

    NASA Technical Reports Server (NTRS)

    Kallman, Tim; Bautista, M.; Palmeri, P.

    2007-01-01

    This viewgraph document reviews the atomic calculations and the measurements from the laboratory that are relevant to our understanding of X-Ray Warm Absorbers. Included is a brief discussion of the theoretical and the experimental tools. Also included is a discussion of the challenges, and calculations relevant to dielectronic recombination, photoionization cross sections, and collisional ionization. A review of the models is included, and the sequence that the models were applied.

  17. Feasibility study of Compton cameras for x-ray fluorescence computed tomography with humans

    NASA Astrophysics Data System (ADS)

    Vernekohl, Don; Ahmad, Moiz; Chinn, Garry; Xing, Lei

    2016-12-01

    X-ray fluorescence imaging is a promising imaging technique able to depict the spatial distributions of low amounts of molecular agents in vivo. Currently, the translation of the technique to preclinical and clinical applications is hindered by long scanning times as objects are scanned with flux-limited narrow pencil beams. The study presents a novel imaging approach combining x-ray fluorescence imaging with Compton imaging. Compton cameras leverage the imaging performance of XFCT and abolish the need for pencil beam excitation. The study examines the potential of this new imaging approach on the base of Monte-Carlo simulations. In the work, it is first presented that the particular option of slice/fan-beam x-ray excitation has advantages in image reconstruction in regard of processing time and image quality compared to traditional volumetric Compton imaging. In a second experiment, the feasibility of the approach for clinical applications with tracer agents made from gold nano-particles is examined in a simulated lung scan scenario. The high energy of characteristic x-ray photons from gold is advantageous for deep tissue penetration and has lower angular blurring in the Compton camera. It is found that Doppler broadening in the first detector stage of the Compton camera adds the largest contribution on the angular blurring; physically limiting the spatial resolution. Following the analysis of the results from the spatial resolution test, resolutions in the order of one centimeter are achievable with the approach in the center of the lung. The concept of Compton imaging allows one to distinguish to some extent between scattered photons and x-ray fluorescent photons based on their difference in emission position. The results predict that molecular sensitivities down to 240 pM l-1 for 5 mm diameter lesions at 15 mGy for 50 nm diameter gold nano-particles are achievable. A 45-fold speed up time for data acquisition compared to traditional pencil beam XFCT could

  18. Optimized acquisition time for x-ray fluorescence imaging of gold nanoparticles: a preliminary study using photon counting detector

    NASA Astrophysics Data System (ADS)

    Ren, Liqiang; Wu, Di; Li, Yuhua; Chen, Wei R.; Zheng, Bin; Liu, Hong

    2016-03-01

    X-ray fluorescence (XRF) is a promising spectroscopic technique to characterize imaging contrast agents with high atomic numbers (Z) such as gold nanoparticles (GNPs) inside small objects. Its utilization for biomedical applications, however, is greatly limited to experimental research due to longer data acquisition time. The objectives of this study are to apply a photon counting detector array for XRF imaging and to determine an optimized XRF data acquisition time, at which the acquired XRF image is of acceptable quality to allow the maximum level of radiation dose reduction. A prototype laboratory XRF imaging configuration consisting of a pencil-beam X-ray and a photon counting detector array (1 × 64 pixels) is employed to acquire the XRF image through exciting the prepared GNP/water solutions. In order to analyze the signal to noise ratio (SNR) improvement versus the increased exposure time, all the XRF photons within the energy range of 63 - 76KeV that include two Kα gold fluorescence peaks are collected for 1s, 2s, 3s, and so on all the way up to 200s. The optimized XRF data acquisition time for imaging different GNP solutions is determined as the moment when the acquired XRF image just reaches a quality with a SNR of 20dB which corresponds to an acceptable image quality.

  19. Analysis of nuclear materials by energy dispersive x-ray fluorescence and spectral effects of alpha decay

    SciTech Connect

    Worley, Christopher G

    2009-01-01

    Energy dispersive X-ray fluorescence (EDXRF) spectra collected from alpha emitters are complicated by artifacts inherent to the alpha decay process, particularly when using portable instruments. For example, {sup 239}Pu EDXRF spectra exhibit a prominent uranium L X-ray emission peak series due to sample alpha decay rather than source-induced X-ray fluorescence. A portable EDXRF instrument was used to collect spectra from plutonium, americium, and a Pu-contaminated steel sample. The plutonium sample was also analyzed by wavelength dispersive XRF to demonstrate spectral differences observed when using these very different instruments.

  20. Uncertainty calculations for the measurement of in vivo bone lead by x-ray fluorescence.

    PubMed

    O'Meara, J M; Fleming, D E B

    2009-04-21

    In order to quantify the bone lead concentration from an in vivo x-ray fluorescence measurement, typically two estimates of the lead concentration are determined by comparing the normalized x-ray peak amplitudes from the Kalpha(1) and Kbeta(1) features to those of the calibration phantoms. In each case, the normalization consists of taking the ratio of the x-ray peak amplitude to the amplitude of the coherently scattered photon peak in the spectrum. These two Pb concentration estimates are then used to determine the weighted mean lead concentration of that sample. In calculating the uncertainties of these measurements, it is important to include any covariance terms where appropriate. When determining the uncertainty of the lead concentrations from each x-ray peak, the standard approach does not include covariance between the x-ray peaks and the coherently scattered feature. These spectral features originate from two distinct physical processes, and therefore no covariance between these features can exist. Through experimental and simulated data, we confirm that there is no observed covariance between the detected Pb x-ray peaks and the coherently scattered photon signal, as expected. This is in direct contrast to recent work published by Brito (2006 Phys. Med. Biol. 51 6125-39). There is, however, covariance introduced in the calculation of the weighted mean lead concentration due to the common coherent normalization. This must be accounted for in calculating the uncertainty of the weighted mean lead concentration, as is currently the case. We propose here an alternative approach to calculating the weighted mean lead concentration in such a way as to eliminate the covariance introduced by the common coherent normalization. It should be emphasized that this alternative approach will only apply in situations in which the calibration line intercept is not included in the calculation of the Pb concentration from the spectral data: when the source of the intercept is

  1. [Application of in situ micro energy dispersive X-ray fluorescence analysis in mineralogy].

    PubMed

    Yang, Hai; Ge, Liang-Quan; Gu, Yi; Zhang, Qing-Xian; Xiong, Sheng-Qing

    2013-11-01

    Thirteen rock samples were collected for studying the variation of element content in the mineral during the alteration process from Xinjiang, China. The IED-6000 in situ micro energy dispersive X-ray fluorescence developed by CDUT was applied to get chemical and physical data from minerals. The non-destructive spectrometer is based on a low-power Mo-anode X-ray tube and a Si-PIN peltier cooled X-ray detector. The unique design of the tube's probe allows very close coupling of polycapillary and makes the use of micro-area measurement feasible and efficient. The spectrometer can be integrated into any microscope for analysis. The long axis diameter of beam spot is about 110 microm. According to micro-EDXRF measurement, the tetrahedrite was corrected to pyrite, improving the efficiency and accuracy of the mineral identification. The feldspar of mineralized rock sample is rich in Cu and Zn which can be used as prospecting indicator elements. Element content of Cr, Mn and Co shows negative correlation with the degree of mineralization.

  2. Phase-resolved x-ray ferromagnetic resonance measurements in fluorescence yield

    SciTech Connect

    Marcham, M. K.; Keatley, P. S.; Neudert, A.; Hicken, R. J.; Cavill, S. A.; Shelford, L. R.; van der Laan, G.; Telling, N. D.; Childress, J. R.; Katine, J. A.; Shafer, P.; Arenholz, E.

    2010-10-14

    Phase-resolved x-ray ferromagnetic resonance (XFMR) has been measured in fluorescence yield, extending the application of XFMR to opaque samples on opaque substrates. Magnetization dynamics were excited in a Co{sub 50}Fe{sub 50}(0.7)/Ni{sub 90}Fe{sub 10}(5) bilayer by means of a continuous wave microwave excitation, while x-ray magnetic circular dichroism (XMCD) spectra were measured stroboscopically at different points in the precession cycle. By tuning the x-ray energy to the L{sub 3} edges of Ni and Fe, the dependence of the real and imaginary components of the element specific magnetic susceptibility on the strength of an externally applied static bias field was determined. First results from measurements on a Co{sub 50}Fe{sub 50}(0.7)/Ni{sub 90}Fe{sub 10}(5)/Dy(1) sample confirm that enhanced damping results from the addition of the Dy cap.

  3. Proton-induces and x-ray induced fluorescence analysis of scoliotic tissue

    SciTech Connect

    Panessa-Warren, B J; Kraner, H W; Jones, K W; Weiss, L S

    1980-02-01

    Adolescent idiopathic scoliosis is characterized by a curvature or assymetry of the spine which may become progressively more severe, with clinical symptoms appearing just prior to, or during, puberty. The incidence for scoliosis in the age group from 12 to 14 years of age has been reported as high as 8 to 10%, with more than 80% of the cases occurring in females. Although pathologic changes exist in muscles from both sides of the spinal curvature, and no statistically significant side differences have been reported, morphologic changes suggest that the concanve side is the most affected. This paper reports our preliminary data on the elemental composition of individual muscle fibers derived from convex, concave and gluteal scoliotic muscle, and erythrocytes from scoliotic and normal patients, analyzed by proton induced x-ray emission (PIXE) and x-ray fluorescence spectroscopy (XRF). A new type of specimen holder was designed for this study which offers low x-ray background, minimal absorption and maintenance of a moist environment around the specimen.

  4. Development of Ta-based Superconducting Tunnel Junction X-ray Detectors for Fluorescence XAS

    SciTech Connect

    Friedrich, S; Drury, O; Hall, J; Cantor, R

    2009-09-23

    We are developing superconducting tunnel junction (STJ) soft X-ray detectors for chemical analysis of dilute samples by fluorescence-detected X-ray absorption spectroscopy (XAS). Our 36-pixel Nb-based STJ spectrometer covers a solid angle {Omega}/4{pi} {approx} 10{sup -3}, offers an energy resolution of {approx}10-20 eV FWHM for energies up to {approx}1 keV, and can be operated at total count rates of {approx}10{sup 6} counts/s. For increased quantum efficiency and cleaner response function, we have now started the development of Ta-based STJ detector arrays. Initial devices modeled after our Nb-based STJs have an energy resolution below 10 eV FWHM for X-ray energies below 1 keV, and pulse rise time discrimination can be used to improve their response function for energies up to several keV. We discuss the performance of the Ta-STJs and outline steps towards the next-generation of large STJ detector arrays with higher sensitivity.

  5. Development of Ta-based Superconducting Tunnel Junction X-ray Detectors for Fluorescence XAS

    SciTech Connect

    Friedrich, Stephan; Drury, Owen B.; Hall, John; Cantor, Robin

    2010-06-23

    We are developing superconducting tunnel junction (STJ) soft X-ray detectors for chemical analysis of dilute samples by fluorescence-detected X-ray absorption spectroscopy (XAS). Our 36-pixel Nb-based STJ spectrometer covers a solid angle {Omega}/4{pi}{approx_equal}10{sup -3}, offers an energy resolution of {approx}10-20 eV FWHM for energies up to {approx}1 keV, and can be operated at total count rates of {approx}10{sup 6} counts/s. For increased quantum efficiency and cleaner response function, we have now started the development of Ta-based STJ detector arrays. Initial devices modeled after our Nb-based STJs have an energy resolution below 10 eV FWHM for X-ray energies below 1 keV, and pulse rise time discrimination can be used to improve their response function for energies up to several keV. We discuss the performance of the Ta-STJs and outline steps towards the next-generation of large STJ detector arrays with higher sensitivity.

  6. Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.

    1989-01-01

    Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

  7. X-ray fluorescence analysis of iron and manganese distribution in primary dopaminergic neurons

    PubMed Central

    Dučić, Tanja; Barski, Elisabeth; Salome, Murielle; Koch, Jan C; Bähr, Mathias; Lingor, Paul

    2013-01-01

    Transition metals have been suggested to play a pivotal role in the pathogenesis of Parkinson's disease. X-ray microscopy combined with a cryogenic setup is a powerful method for elemental imaging in low concentrations and high resolution in intact cells, eliminating the need for fixation and sectioning of the specimen. Here, we performed an elemental distribution analysis in cultured primary midbrain neurons with a step size in the order of 300 nm and ∼ 0.1 ppm sensitivity under cryo conditions by using X-ray fluorescence microscopy. We report the elemental mappings on the subcellular level in primary mouse dopaminergic (DAergic) and non-DAergic neurons after treatment with transition metals. Application of Fe2+ resulted in largely extracellular accumulation of iron without preference for the neuronal transmitter subtype. A quantification of different Fe oxidation states was performed using X-ray absorption near edge structure analysis. After treatment with Mn2+, a cytoplasmic/paranuclear localization of Mn was observed preferentially in DAergic neurons, while no prominent signal was detectable after Mn3+ treatment. Immunocytochemical analysis correlated the preferential Mn uptake to increased expression of voltage-gated calcium channels in DAergic neurons. We discuss the implications of this differential elemental distribution for the selective vulnerability of DAergic neurons and Parkinson's disease pathogenesis. PMID:23106162

  8. Non-destructive in situ study of "Mad Meg" by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Van Pevenage, Jolien; De Langhe, Kaat; De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo; Vandenabeele, Peter; Martens, Maximiliaan P. J.

    2014-07-01

    "Mad Meg", a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO2 + 15% K2O + 10% CoO + 5% Al2O3) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel.

  9. Microwave-assisted synthesis of water-soluble, fluorescent gold nanoclusters capped with small organic molecules and a revealing fluorescence and X-ray absorption study

    NASA Astrophysics Data System (ADS)

    Helmbrecht, C.; Lützenkirchen-Hecht, D.; Frank, W.

    2015-03-01

    Colourless solutions of blue light-emitting, water-soluble gold nanoclusters (AuNC) were synthesized from gold colloids under microwave irradiation using small organic molecules as ligands. Stabilized by 1,3,5-triaza-7-phosphaadamantane (TPA) or l-glutamine (GLU), fluorescence quantum yields up to 5% were obtained. AuNC are considered to be very promising for biological labelling, optoelectronic devices and light-emitting materials but the structure-property relationships have still not been fully clarified. To expand the knowledge about the AuNC apart from their fluorescent properties they were studied by X-ray absorption spectroscopy elucidating the oxidation state of the nanoclusters' gold atoms. Based on curve fitting of the XANES spectra in comparison to several gold references, optically transparent fluorescent AuNC are predicted to be ligand-stabilized Au5+ species. Additionally, their near edge structure compared with analogous results of polynuclear clusters known from the literature discloses an increasing intensity of the feature close to the absorption edge with decreasing cluster size. As a result, a linear relationship between the cluster size and the X-ray absorption coefficient can be established for the first time.Colourless solutions of blue light-emitting, water-soluble gold nanoclusters (AuNC) were synthesized from gold colloids under microwave irradiation using small organic molecules as ligands. Stabilized by 1,3,5-triaza-7-phosphaadamantane (TPA) or l-glutamine (GLU), fluorescence quantum yields up to 5% were obtained. AuNC are considered to be very promising for biological labelling, optoelectronic devices and light-emitting materials but the structure-property relationships have still not been fully clarified. To expand the knowledge about the AuNC apart from their fluorescent properties they were studied by X-ray absorption spectroscopy elucidating the oxidation state of the nanoclusters' gold atoms. Based on curve fitting of the XANES

  10. [Establishment and Improvement of Portable X-Ray Fluorescence Spectrometer Detection Model Based on Wavelet Transform].

    PubMed

    Li, Fang; Wang, Ji-hua; Lu, An-xiang; Han, Ping

    2015-04-01

    The concentration of Cr, Cu, Zn, As and Pb in soil was tested by portable X-ray fluorescence spectrometer. Each sample was tested for 3 times, then after using wavelet threshold noise filtering method for denoising and smoothing the spectra, a standard curve for each heavy metal was established according to the standard values of heavy metals in soil and the corresponding counts which was the average of the 3 processed spectra. The signal to noise ratio (SNR), mean square error (MSE) and information entropy (H) were taken to assess the effects of denoising when using wavelet threshold noise filtering method for determining the best wavelet basis and wavelet decomposition level. Some samples with different concentrations and H3 B03 (blank) were chosen to retest this instrument to verify its stability. The results show that: the best denoising result was obtained with the coif3 wavelet basis at the decomposition level of 3 when using the wavelet transform method. The determination coefficient (R2) range of the instrument is 0.990-0.996, indicating that a high degree of linearity was found between the contents of heavy metals in soil and each X-ray fluorescence spectral characteristic peak intensity with the instrument measurement within the range (0-1,500 mg · kg(-1)). After retesting and calculating, the results indicate that all the detection limits of the instrument are below the soil standards at national level. The accuracy of the model has been effectively improved, and the instrument also shows good precision with the practical application of wavelet transform to the establishment and improvement of X-ray fluorescence spectrometer detection model. Thus the instrument can be applied in on-site rapid screening of heavy metal in contaminated soil.

  11. Total reflection X-ray fluorescence spectrometers for multielement analysis: status of equipment

    NASA Astrophysics Data System (ADS)

    Ayala Jiménez, Rony E.

    2001-11-01

    Multielement analysis by total reflection X-ray fluorescence spectrometry has evolved during two decades. At present commercial equipment is available for chemical analysis of all types of biological and mineral samples. The electronic industry has also benefited from scientific and technological developments in this field due to new instrumentation to determine contamination on the surface of silicon wafers (the equipment will not be covered in this paper). The basic components of the spectrometers can be summarized as follows: (a) excitation source; (b) geometric arrangement (optics) for collimation and monochromatization of the primary radiation; (c) X-ray detector; and (d) software for operation of the instrument, data acquisition and spectral deconvolution to determine the concentrations of the elements (quantitative analysis). As an optional feature one manufacturer offers a conventional 45° geometry for direct excitation. Personal communications of the author and commercial brochures available have allowed us to list the components used in TXRF for multielement analysis. Excitation source: high-power sealed X-ray tubes, output from 1300 to 3000 W, different mixed alloy anodes Mo/W are used but molybdenum, tungsten and copper are common; single anode metal ceramic low power X-ray tubes, output up to 40 W. Excitation systems can be customized according to the requirements of the laboratory. Detector: silicon-lithium drifted semiconductor detector liquid nitrogen cooled; or silicon solid state thermoelectrically cooled detector (silicon drift detector SDD and silicon-PIN diode detector). Optics: multilayer monochromator of silicon-tungsten, nickel-carbon or double multilayer monochromator. Electronics: spectroscopy amplifier, analog to digital converter adapted to a PC compatible computer with software in a Windows environment for the whole operation of the spectrometer and for qualitative/quantitative analysis of samples are standard features in the

  12. Hyper-filter-fluorescer spectrometer for x-rays above 120 keV

    DOEpatents

    Wang, Ching L.

    1983-01-01

    An apparatus utilizing filter-fluorescer combinations is provided to measure short bursts of high fluence x-rays above 120 keV energy, where there are no practical absorption edges available for conventional filter-fluorescer techniques. The absorption edge of the prefilter is chosen to be less than that of the fluorescer, i.e., E.sub.PRF E.sub.F. In this way, the response function is virtually zero between E.sub.PRF and E.sub.F and well defined and enhanced in an energy band of less than 1000 keV above the 120 keV energy.

  13. Imaging x-ray fluorescence relevant to hydrodynamic mixing experiments at the National Ignition Facility

    NASA Astrophysics Data System (ADS)

    MacDonald, Michael; Gamboa, Eliseo; Kuranz, Carolyn; Keiter, Paul; Drake, R. Paul

    2012-10-01

    The National Ignition Facility (NIF) is capable of providing enough energy to explore areas of physics that are not possible on any previous laser system. This includes large-volume, geometrically complex hydrodynamic and radiation hydrodynamic experiments in which traditional, line-integrated radiographic techniques limit the quality of the results. As an example, we are involved in divergent hydrodynamic experiments at the NIF, motivated by supernova hydrodynamics, that cannot be diagnosed in detail with transmission radiography. X-ray scattering has been considered for this purpose and appears feasible [1]. Here we consider fluorescence imaging, a better candidate as the cross section of photoabsorption in the several-keV range is roughly 100 times larger than that of scattering. A single layer of the target will be uniformly doped with a fluorescent tracer, which will be pumped by a sheet of x-rays. The fluorescent intensity will be measured to create a density map of the doped material as it mixes with other layers. Developing this diagnostic will create a powerful tool to characterize hydrodynamic experiments with complex geometries.[4pt] [1] Huntington et al. High Energy Density Physics 6, 194 (2010).

  14. The Bionanoprobe: hard X-ray fluorescence nanoprobe with cryogenic capabilities

    PubMed Central

    Chen, S.; Deng, J.; Yuan, Y.; Flachenecker, C.; Mak, R.; Hornberger, B.; Jin, Q.; Shu, D.; Lai, B.; Maser, J.; Roehrig, C.; Paunesku, T.; Gleber, S. C.; Vine, D. J.; Finney, L.; VonOsinski, J.; Bolbat, M.; Spink, I.; Chen, Z.; Steele, J.; Trapp, D.; Irwin, J.; Feser, M.; Snyder, E.; Brister, K.; Jacobsen, C.; Woloschak, G.; Vogt, S.

    2014-01-01

    Hard X-ray fluorescence microscopy is one of the most sensitive techniques for performing trace elemental analysis of biological samples such as whole cells and tissues. Conventional sample preparation methods usually involve dehydration, which removes cellular water and may consequently cause structural collapse, or invasive processes such as embedding. Radiation-induced artifacts may also become an issue, particularly as the spatial resolution increases beyond the sub-micrometer scale. To allow imaging under hydrated conditions, close to the ‘natural state’, as well as to reduce structural radiation damage, the Bionanoprobe (BNP) has been developed, a hard X-ray fluorescence nanoprobe with cryogenic sample environment and cryo transfer capabilities, dedicated to studying trace elements in frozen-hydrated biological systems. The BNP is installed at an undulator beamline at sector 21 of the Advanced Photon Source. It provides a spatial resolution of 30 nm for two-dimensional fluorescence imaging. In this first demonstration the instrument design and motion control principles are described, the instrument performance is quantified, and the first results obtained with the BNP on frozen-hydrated whole cells are reported. PMID:24365918

  15. Use of X-ray Fluorescence Analysis for the Determination of Rare Earth Elements

    NASA Astrophysics Data System (ADS)

    Schramm, Rainer

    2016-09-01

    X-ray fluorescence spectrometry (XRF) is a powerful tool for the analysis of solid material. That is the reason why the technique was applied for the determination of rare earth elements (REEs) since about 1970. At present, energy-dispersive XRF and wavelength-dispersive XRF are used for the analysis of pressed powder pellets or fused Li-borate beads containing REEs. The production of reliable results can only be achieved by careful optimization of the parameter, in particular the selection of spectral lines. The quantification is based on a calibration realized by using reference samples.

  16. Combined backscatter Moessbauer spectrometer/x ray fluorescence analyzer (BaMS/XRF) for extraterrestrial surfaces

    NASA Technical Reports Server (NTRS)

    Shelfer, T. D.; Wills, E. L.; Agresti, D. G.; Pimperl, M. M.; Shen, M. H.; Morris, R. V.; Nguyen, T.

    1993-01-01

    We have designed and tested a prototype combined backscatter Moessbauer spectrometer and x-ray fluorescence analyzer (BaMS/XRF). A space qualified instrument based on this design would be suitable for in-situ use on planetary missions to the surfaces of the Moon (Artemis and lunar outpost), Mars (MESUR), asteroids, or other solid solar system objects. The BaMS/XRF instrument is designed to be capable of concurrent sample analyses for the mineralogy of iron-bearing phases and elemental composition without the need for sample preparation.

  17. Determination of Yttrium in High Density Silicon Nitride by Emission and X-Ray Fluorescence Spectroscopy.

    DTIC Science & Technology

    1981-08-01

    AD-AI07 596 ARMY MATERIALS AND MECHANICS RESEARCH CENTER WATERTOWN MA F/S 7/4 DETERMINATION OF YTTRIUM IN HIGH DENSITY SILICON NITRIDE BY EMI-ETCIU...AUG Al B H STRAUSS. UNCLASSIFIED AMMRC-TR-Al-39 N AMMRC TR 81-39 A ~LEVEL ’ t’- .- DETERMINATION OF YTTRIUM IN 1 HIGH DENSITY SILICON NITRIDE BY...DETERMINATION OF YTTRIUM IN HIGH DENSITY SILICON NITRIDE BY EMISSION AND X-RAY Final Report FLUORESCENCE SPECTROSCOPY 6 PERFORMING ORG. REPORT NUMBER 7. AUTHOR

  18. Preliminary testing of a prototype portable X-ray fluorescence spectrometer

    NASA Technical Reports Server (NTRS)

    Patten, L. L.; Anderson, N. B.; Stevenson, J. J.

    1982-01-01

    A portable X-ray fluorescence spectrometer for use as an analyzer in mineral resource investigative work was built and tested. The prototype battery powered spectrometer, measuring 11 by 12 by 5 inches and weighing only about 15 pounds, was designed specifically for field use. The spectrometer has two gas proportional counters and two radioactive sources, Cd (10a) and Fe (55). Preliminary field and laboratory tests on rock specimens and rock pulps have demonstrated the capability of the spectrometer to detect 33 elements to date. Characteristics of the system present some limitations, however, and further improvements are recommended.

  19. The determination of nanogram amounts of Chromium in urine by x-ray fluorescence spectroscopy

    USGS Publications Warehouse

    Beyermann, K.; Rose, H.J.; Christian, R.P.

    1969-01-01

    Nanogram amounts of chromium can be extracted as oxinate into chloform. By treatment of the chloroform layer 3 M hydrochloric acid, oxinates of other elements and excess of reagent are removed, leaving a chloroform solution of the chromium chelate only. This solution is concentrated and transferred to the top of a small brass rod acting as sample holder. The intensity of the X-ray fluorescence of the Cr K?? line is measured with curved crystal optics. Chromium amounts greater than 5 ng can be detected. The application of the procedure to the analysis of the chromium content of urine is demonstrated. ?? 1969.

  20. Analysis Results for Lunar Soil Simulant Using a Portable X-Ray Fluorescence Analyzer

    NASA Technical Reports Server (NTRS)

    Boothe, R. E.

    2006-01-01

    Lunar soil will potentially be used for oxygen generation, water generation, and as filler for building blocks during habitation missions on the Moon. NASA s in situ fabrication and repair program is evaluating portable technologies that can assess the chemistry of lunar soil and lunar soil simulants. This Technical Memorandum summarizes the results of the JSC 1 lunar soil simulant analysis using the TRACeR III IV handheld x-ray fluorescence analyzer, manufactured by KeyMaster Technologies, Inc. The focus of the evaluation was to determine how well the current instrument configuration would detect and quantify the components of JSC-1.

  1. Synchrotron based X-ray fluorescence activities at Indus-2: An overview

    SciTech Connect

    Tiwari, M. K.

    2014-04-24

    X-Ray fluorescence (XRF) spectrometry is a powerful non-destructive technique for elemental analysis of materials at bulk and trace concentration levels. Taking into consideration several advantages of the synchrotron based XRF technique and to fulfill the requirements of Indian universities users we have setup a microfocus XRF beamline (BL-16) on Indus-2 synchrotron light source. The beamline offers a wide range of usages – both from research laboratories and industries; and for researchers working in diverse fields. A brief overview of the measured performance of the beamline, design specifications including various attractive features and recent research activities carried out on the BL-16 beamline are presented.

  2. Application of energy dispersive X-ray fluorescence spectrometry (EDX) in a case of methomyl ingestion.

    PubMed

    Kinoshita, Hiroshi; Tanaka, Naoko; Jamal, Mostofa; Kumihashi, Mitsuru; Okuzono, Ryota; Tsutsui, Kunihiko; Ameno, Kiyoshi

    2013-04-10

    We applied energy dispersive X-ray fluorescence spectrometry (EDX) in a case of poisoning by methomyl, a carbamate pesticide. Quantitative GC/MS analysis showed that the concentration of methomyl-oxime in the femoral blood was 4.0 μg/ml. The elemental analysis by EDX identified the high peak of silicon and sulfur in the stomach contents. We concluded that the cause of his death was methomyl poisoning. This indicates that screening of stomach contents by EDX provides useful information for the forensic diagnosis.

  3. An x-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation.

    SciTech Connect

    Alatas, A.; Alp, E. E.; Friedman, E. S.; Jennings, G.; Johnson, C. E.; Lai, B.; Mini, S. M.; Sato, Y.; Wilkinson, T. J.; Yener, K. A.

    1999-03-10

    Sediments from relic Lake Golbasi were analyzed by X-ray fluorescence with synchrotrons radiation to determine changes in element concentrations over time with selected elements serving as proxies for environmental change. Increases in Ca and Sr suggest soil formation during a dry period, from ca. 4500 BC to ca. 200 AD at which point K, Rb, Zr, Ti, and Y increase, indicating the return of a wet environment. Soil erosion, represented by Cr and Ni, increases ca. 7000 BC, probably as a consequence of environmental change, prior to suggested exploitation of natural resources by the newly urbanized society of the third millennium BC.

  4. Waste reduction and process improvements in the analysis of plutonium by x-ray fluorescence

    SciTech Connect

    Worley, Christopher G; Sodweberg, Constance B; Townsend, Lisa E

    2009-01-01

    Significant modifications were made to a sample preparation process for quantifying gallium in plutonium metal by wavelength dispersive X-ray fluorescence. These changes were made to minimize waste and improve process safety and efficiency. Sample sizes were reduced, cheaper sample preparation acids were used, and safety improvements were implemented. Using this modified process, results from analyzing a batch oftest samples indicated that relative precision and accuracy were {approx}0.2% and {approx}0.1% respectively, which is comparable to that obtained using the older, established sample preparation method.

  5. [Radionuclide X-ray fluorescence as an alternative method to pharmacopeial tests for heavy metals].

    PubMed

    Jánosová, V; Sýkorová, M; Stroffeková, O; Havránek, E

    2006-09-01

    Pharmacopeial tests for heavy metals require comparisons between test solution's colour after addition of thioacetamide and a control solution containing a known quantity of Pb. As this test neither informs about the type of heavy metals, nor about the concentrations of each of them, there is a reason for more frequent employment of instrumental methods such as AAS and AES, as well as ICP, NAA, and X-ray fluorescence. These methods provide us with quick and exact elemental analyses of impurities, thus becoming more and more important in the quality control of drugs and medicinal plants.

  6. Corrections for matrix effects in X-ray fluorescence analysis—A tutorial

    NASA Astrophysics Data System (ADS)

    Rousseau, Richard M.

    2006-07-01

    This paper presents the basic concepts of the mathematical correction for matrix effects in X-ray fluorescence analysis. The emphasis is placed on the correction factor for matrix effects and its quantification. This correction factor is calculated using mathematical models proposed by Lachance-Traill, Claisse-Quintin and Rousseau, which can be applied in practice via an efficient calibration procedure. Each variable in these models is clearly identified so that specific numerical values can easily be substituted for calculation. This paper describes and emphasizes the application of the most effective existing models.

  7. In-Situ Silver Acetylide Silver Nitrate Explosive Deposition Measurements Using X-Ray Fluorescence.

    SciTech Connect

    Covert, Timothy Todd

    2014-09-01

    The Light Initiated High Explosive facility utilized a spray deposited coating of silver acetylide - silver nitrate explosive to impart a mechanical shock into targets of interest. A diagnostic was required to measure the explosive deposition in - situ. An X - ray fluorescence spectrometer was deployed at the facility. A measurement methodology was developed to measure the explosive quantity with sufficient accuracy. Through the use of a tin reference material under the silver based explosive, a field calibration relationship has been developed with a standard deviation of 3.2 % . The effect of the inserted tin material into the experiment configuration has been explored.

  8. Determination of metals in lubricating oils by X-ray fluorescence spectrometry.

    PubMed

    Pouzar, M; Cernohorský, T; Krejcová, A

    2001-06-21

    The determination of common wear metals, namely iron, chromium, copper, zinc and lead, in a wide range of lubricating oil samples was investigated for the use of a low-cost, wavelength-dispersive X-ray fluorescence spectrometer. The procedure provided results in satisfactory agreement with inductively coupled plasma spectrometry used as reference method after microwave digestion of the samples in concentrated nitric acid. Statistical tests following extensive regression analyses of the data indicated that interelement effects were not statistically significant and that a simple linear regression was adequate for the calibration of individual metals.

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

    NASA Astrophysics Data System (ADS)

    Borgese, Laura; Bilo, Fabjola; Tsuji, Kouichi; Fernández-Ruiz, Ramón; Margui, Eva; Streli, Christina; Pepponi, Giancarlo; Stosnach, Hagen; Yamada, Takashi; Vandenabeele, Peter; Maina, David M.; Gatari, Michael; Shepherd, Keith D.; Towett, Erick K.; Bennun, Leonardo; Custo, Graciela; Vasquez, Cristina; Depero, Laura E.

    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.

  10. Analysis of obsidian artifacts in Southern Meso-America using x-ray fluorescence

    SciTech Connect

    Nelson, F.W.

    1996-12-31

    The analysis of obsidian artifacts using X-ray fluorescence (XRF) spectrometry has been an important tool for archaeologists for {approximately}25 yr. However, as methods and instrumentation have improved, more reliable information regarding exchange and routes of exchange has been obtained. In southern Meso-America, obsidian analyses have demonstrated changes in the obsidian geologic sources used by prehistoric peoples through time. These changes in sources of obsidian have been used to describe possible changes of prehistoric trade routes. The methods and results of analysis are described in this paper.

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

    SciTech Connect

    Tiwari, M. K. Singh, A. K. Das, Gangadhar Chowdhury, Anupam Lodha, G. S.

    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.

  12. Lead nephropathy: In vivo x ray fluorescence (XRF) for assessing body lead stores

    SciTech Connect

    Wedeen, R.P.; Batuman, V.; Quinless, F.; Williams, F.H. Jr.; Bogden, J.; Schidlovsky, G.; Jones, K.W.

    1986-01-01

    The EDTA lead mobilization test has proven of value in the diagnosis of renal disease due to lead (lead nephropathy) but is unsuitable for large scale studies in patients with end-stage renal disease. A rapid, safe, non-invasive technique for determining body lead stores by in vivo tibial x ray fluorescence (XRF) is described. These studies show that the chelation test can be replaced by in vivo XRF in patients with end-stage renal disease. XRF, for the first time, will permit epidemiologic studies of large populations which may be at risk for lead nephropathy from excessive exposure to environmental lead. 15 refs., 2 figs.

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

    NASA Astrophysics Data System (ADS)

    Tiwari, M. K.; Singh, A. K.; Das, Gangadhar; Chowdhury, Anupam; Lodha, G. S.

    2014-04-01

    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.

  14. In-vivo Fluorescent X-ray CT Imaging of Mouse Brain

    SciTech Connect

    Takeda, T.; Wu, J.; Lwin, Thet-Thet; Huo, Q.; Minami, M.; Sunaguchi, N.; Murakami, T.; Mouri, S.; Nasukawa, S.; Yuasa, T.; Akatsuka, T.; Hyodo, K.; Hontani, H.

    2007-01-19

    Using a non-radioactive iodine-127 labeled cerebral perfusion agent (I-127 IMP), fluorescent X-ray computed tomography (FXCT) clearly revealed the cross-sectional distribution of I-127 IMP in normal mouse brain in-vivo. Cerebral perfusion of cortex and basal ganglion was depicted with 1 mm in-plane spatial resolution and 0.1 mm slice thickness. Degree of cerebral perfusion in basal ganglion was about 2-fold higher than that in cortical regions. This result suggests that in-vivo cerebral perfusion imaging is realized quantitatively by FXCT at high volumetric resolution.

  15. Radioisotope x-ray fluorescence analysis of ancient pottery from Tel Kouzama site in Damascus, Syria.

    PubMed

    Bakraji, Elias Hanna; Romeié, Mouhammad; Issa, Haissam

    2006-01-01

    The radioisotope X-ray fluorescence method has been utilized in the analysis of thirty nine archaeological pottery fragment samples from Tel Kouzama site, Damascus city, Syria. The samples were irradiated by a 109Cd radioisotope source (-9 10(8) Bq) for 1000 s. 17 chemical elements were determined. These elemental concentrations have been processed using two multivariate statistical methods, cluster and factor analysis in order to determine similarities and correlation between the various samples. Factor analysis confirms that samples were correctly classified by cluster analysis. These two methods suggest that samples can be considered to be manufactured using four different sources of raw material.

  16. A new detector system for low energy X-ray fluorescence coupled with soft X-ray microscopy: First tests and characterization

    NASA Astrophysics Data System (ADS)

    Gianoncelli, Alessandra; Bufon, Jernej; Ahangarianabhari, Mahdi; Altissimo, Matteo; Bellutti, Pierluigi; Bertuccio, Giuseppe; Borghes, Roberto; Carrato, Sergio; Cautero, Giuseppe; Fabiani, Sergio; Giacomini, Gabriele; Giuressi, Dario; Kourousias, George; Menk, Ralf Hendrik; Picciotto, Antonino; Piemonte, Claudio; Rachevski, Alexandre; Rashevskaya, Irina; Stolfa, Andrea; Vacchi, Andrea; Zampa, Gianluigi; Zampa, Nicola; Zorzi, Nicola

    2016-04-01

    The last decades have witnessed substantial efforts in the development of several detector technologies for X-ray fluorescence (XRF) applications. In spite of the increasing trend towards performing, cost-effective and reliable XRF systems, detectors for soft X-ray spectroscopy still remain a challenge, requiring further study, engineering and customization in order to yield effective and efficient systems. In this paper we report on the development, first characterization and tests of a novel multielement detector system based on low leakage current silicon drift detectors (SDD) coupled to ultra low noise custom CMOS preamplifiers for synchrotron-based low energy XRF. This new system exhibits the potential for improving the count rate by at least an order of magnitude resulting in ten-fold shorter dwell time at an energy resolution similar to that of single element silicon drift detectors.

  17. Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

    NASA Astrophysics Data System (ADS)

    Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893-972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts.

  18. X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

    NASA Astrophysics Data System (ADS)

    Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

    2011-12-01

    The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I

  19. Extracting material parameters from x-ray attenuation: a CT feasibility study using kilovoltage synchrotron x-rays incident upon low atomic number absorbers.

    PubMed

    Kirby, B J; Davis, J R; Grant, J A; Morgan, M J

    2003-10-21

    The work reported here is a feasibility study of the extraction of material parameters from measurements of the linear x-ray attenuation coefficient of low atomic number absorbers. Computed tomography (CT) scans of small samples containing several liquids and solids were carried out with synchrotron radiation at the Australian National Beamline Facility (BL 20B) in Japan. Average values of the x-ray linear attenuation coefficient were extracted for each material for x-ray energies ranging from 11 keV to 20.5 keV. The electron density was estimated by applying results derived from a parametrization of the x-ray linear attenuation coefficient first developed by Jackson and Hawkes and extended for this work. Average estimates for the electron density of triethanolamine and acetic acid were made to within +5.3% of the actual value. Other materials examined included furfuraldehyde, perspex and teflon, for which average estimates of the electron density were less than 10% in excess of the calculated value.

  20. Breakthrough: X-ray Laser Captures Atoms and Molecules in Action

    ScienceCinema

    Bergmann, Uwe

    2016-07-12

    The Linac Coherent Light Source at SLAC is the world's most powerful X-ray laser. Just two years after turning on in 2009, breakthrough science is emerging from the LCLS at a rapid pace. A recent experiment used the X-rays to create and probe a 2-million-degree piece of matter in a controlled way for the first time-a significant leap toward understanding the extreme conditions found in the hearts of stars and giant planets, and a finding which could further guide research into nuclear fusion, the mechanism that powers the sun. Upcoming experiments will investigate the fundamental, atomic-scale processes behind such phenomena as superconductivity and magnetism, as well as peering into the molecular workings of photosynthesis in plants.

  1. Compton scattering of an X-ray photon by an open-shell atom

    NASA Astrophysics Data System (ADS)

    Hopersky, A. N.; Nadolinsky, A. M.

    2012-09-01

    A nonrelativistic quantum theory for the nonresonant Compton scattering of an X-ray photon by a free many-electron atom with an open shell in the ground state has been constructed in the single-configuration Hartree-Fock approximation outside the impulse approximation widely used in the literature. The transition to an atom with closed shells reproduces the results obtained previously in [6, 7]. The results of a test calculation for atoms with open (Ti, Fe) and closed (Zn) 3 d core shells are presented. The effects of the radial relaxation of one-electron states in the field of core vacancies have been taken into account. The results of the calculation agree well with the experimental results [15, 16]. It has been established that the results of the impulse approximation in the investigated X-ray photon energy ranges disagree with those of our theory not only quantitatively but also qualitatively. In particular, the impulse approximation near the elastic (Thomson and Rayleigh) scattering line leads to a gross overestimation of the contributions from the deep atomic shells involved in the inelastic photon scattering only virtually to the scattering probability. The presented theory is general in character and its applicability to a particular element of the Mendeleev table with an open core shell or to a many-electron atomic ion is limited only by the requirement that the nonrelativistic Hartree-Fock approximation be properly used in describing the scattering-state wave functions.

  2. Compton scattering of an X-ray photon by an open-shell atom

    SciTech Connect

    Hopersky, A. N. Nadolinsky, A. M.

    2012-09-15

    A nonrelativistic quantum theory for the nonresonant Compton scattering of an X-ray photon by a free many-electron atom with an open shell in the ground state has been constructed in the single-configuration Hartree-Fock approximation outside the impulse approximation widely used in the literature. The transition to an atom with closed shells reproduces the results obtained previously in [6, 7]. The results of a test calculation for atoms with open (Ti, Fe) and closed (Zn) 3d core shells are presented. The effects of the radial relaxation of one-electron states in the field of core vacancies have been taken into account. The results of the calculation agree well with the experimental results [15, 16]. It has been established that the results of the impulse approximation in the investigated X-ray photon energy ranges disagree with those of our theory not only quantitatively but also qualitatively. In particular, the impulse approximation near the elastic (Thomson and Rayleigh) scattering line leads to a gross overestimation of the contributions from the deep atomic shells involved in the inelastic photon scattering only virtually to the scattering probability. The presented theory is general in character and its applicability to a particular element of the Mendeleev table with an open core shell or to a many-electron atomic ion is limited only by the requirement that the nonrelativistic Hartree-Fock approximation be properly used in describing the scattering-state wave functions.

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

    NASA Astrophysics Data System (ADS)

    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.

  4. Determination of sulfur and chlorine in fodder by X-ray fluorescence spectral analysis and comparison with other analytical methods

    NASA Astrophysics Data System (ADS)

    Nečemer, Marijan; Kump, Peter; Rajčevič, Marija; Jačimović, Radojko; Budič, Bojan; Ponikvar, Maja

    2003-07-01

    Sulfur and chlorine are essential elements in the metabolic processes of ruminants, and correct planning strategy of ruminant nutrition should provide a sufficient content of S and Cl in the animal's body. S and Cl can be found in various types of animal fodder in the form of organic compounds and minerals. In this work, the Cl and S content in forage was determined by X-ray fluorescence spectrometry (XRF), and its performance was then compared in parallel analyses by instrumental neutron activation analysis (INAA), inductively coupled plasma atomic emission spectrometry (ICP-AES) and potentiometric methods. The results were compared and critically evaluated in order to assess the performance and capability of the XRF technique in analysis of animal fodder.

  5. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

    SciTech Connect

    Wang, Y.; Qun, Y; Ablett, J

    2008-01-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  6. X-ray fluorescence tomography: Jacobin matrix and confidence of the reconstructed images

    NASA Astrophysics Data System (ADS)

    Nikolaev, Dmitry; Chukalina, Marina

    2015-02-01

    The goal of the X-ray Fluorescence Computed Tomography (XFCT) is to give the quantitative description of an object under investigation (sample) in terms of the element composition. However, light and heavy elements inside the object give different contribution to the attenuation of the X-ray probe and of the fluorescence. It leads to the elements got in the shadow area do not give any contribution to the registered spectrum. Iterative reconstruction procedures will try to set to zero the variables describing the element content in composition of corresponding unit volumes as these variables do not change system's condition number. Inversion of the XFCT Radon transform gives random values in these areas. To evaluate the confidence of the reconstructed images we first propose, in addition to the reconstructed images, to calculate a generalized image based on Jacobian matrix. This image highlights the areas of doubt in case if there are exist. In the work we have attempted to prove the advisability of such an approach. For this purpose, we analyzed in detail the process of tomographic projection formation.

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

    NASA Astrophysics Data System (ADS)

    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.

    2014-02-01

    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.

  8. Preparing Adherent Cells for X-ray Fluorescence Imaging by Chemical Fixation

    PubMed Central

    Finney, Lydia A.; Jin, Qiaoling

    2015-01-01

    X-ray fluorescence imaging allows us to non-destructively measure the spatial distribution and concentration of multiple elements simultaneously over large or small sample areas. It has been applied in many areas of science, including materials science, geoscience, studying works of cultural heritage, and in chemical biology. In the case of chemical biology, for example, visualizing the metal distributions within cells allows us to study both naturally-occurring metal ions in the cells, as well as exogenously-introduced metals such as drugs and nanoparticles. Due to the fully hydrated nature of nearly all biological samples, cryo-fixation followed by imaging under cryogenic temperature represents the ideal imaging modality currently available. However, under the circumstances that such a combination is not easily accessible or practical, aldehyde based chemical fixation remains useful and sometimes inevitable. This article describes in as much detail as possible in the preparation of adherent mammalian cells by chemical fixation for X-ray fluorescent imaging. PMID:25867691

  9. [Mapping metal elements of Shuangbai dinosaur fossil by synchrotron X-ray fluorescence microprobe].

    PubMed

    Wang, Yi-Lin; Yang, Qun; Ablett, J M

    2008-05-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is ture for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  10. Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

    NASA Astrophysics Data System (ADS)

    Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

    Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

  11. Time-resolved measurements of short-wavelength fluorescence from x-ray-excited ions.

    PubMed

    Kapteyn, H C; Murnane, M M; Falcone, R W

    1987-09-01

    We demonstrate a novel technique for time-resolved spectroscopic studies of highly excited ions. The technique uses a laser-produced plasma as a short-pulse, soft-x-ray light source with a high repetition rate. A Nd:YAG laser with a pulse duration of 90 psec, a pulse energy of 70 microJ, and repetition rate of 10(4) pulses per second is focused onto a rotating metal target. Soft x rays from the resulting plasma photoionize a gas surrounding the target, and fluorescence from the gas is detected by using a spectrometer and a high-speed photodetector. Using the technique of time-correlated photon counting, we determined the radiative lifetime and collisional quenching rate of the Xe III 5s(0)5p(6)(1)S(0) state by observing its fluorescence at 108.9 nm. A time resolution of better than 400 psec was obtained. We also measured relative Auger decay yields of a core hole state in xenon using a higher-energy laser-produced plasma light source at a lower repetition rate.

  12. Imaging of intracellular fatty acids by scanning X-ray fluorescence microscopy

    PubMed Central

    Shimura, Mari; Shindou, Hideo; Szyrwiel, Lukasz; Tokuoka, Suzumi M.; Hamano, Fumie; Matsuyama, Satoshi; Okamoto, Mayumi; Matsunaga, Akihiro; Kita, Yoshihiro; Ishizaka, Yukihito; Yamauchi, Kazuto; Kohmura, Yoshiki; Lobinski, Ryszard; Shimizu, Isao; Shimizu, Takao

    2016-01-01

    Fatty acids are taken up by cells and incorporated into complex lipids such as neutral lipids and glycerophospholipids. Glycerophospholipids are major constituents of cellular membranes. More than 1000 molecular species of glycerophospholipids differ in their polar head groups and fatty acid compositions. They are related to cellular functions and diseases and have been well analyzed by mass spectrometry. However, intracellular imaging of fatty acids and glycerophospholipids has not been successful due to insufficient resolution using conventional methods. Here, we developed a method for labeling fatty acids with bromine (Br) and applied scanning X-ray fluorescence microscopy (SXFM) to obtain intracellular Br mapping data with submicrometer resolution. Mass spectrometry showed that cells took up Br-labeled fatty acids and metabolized them mainly into glycerophospholipids in CHO cells. Most Br signals observed by SXFM were in the perinuclear region. Higher resolution revealed a spot-like distribution of Br in the cytoplasm. The current method enabled successful visualization of intracellular Br-labeled fatty acids. Single-element labeling combined with SXFM technology facilitates the intracellular imaging of fatty acids, which provides a new tool to determine dynamic changes in fatty acids and their derivatives at the single-cell level.—Shimura, M., Shindou, H., Szyrwiel, L., Tokuoka, S. M., Hamano, F., Matsuyama, S., Okamoto, M., Matsunaga, A., Kita, Y., Ishizaka, Y., Yamauchi, K., Kohmura, Y., Lobinski, R., Shimizu, I., Shimizu, T. Imaging of intracellular fatty acids by scanning X-ray fluorescence microscopy. PMID:27601443

  13. A robust X-ray fluorescence technique for multielemental analysis of solid samples.

    PubMed

    Kallithrakas-Kontos, Nikolaos; Foteinis, Spyros; Paigniotaki, Katherine; Papadogiannakis, Minos

    2016-02-01

    X-ray fluorescence (XRF) quantitation software programs are widely used for analyzing environmental samples due to their versatility but at the expense of accuracy. In this work, we propose an accurate, robust, and versatile technique for multielemental X-ray fluorescence analytical applications, by spiking solid matrices with standard solutions. National Institute of Standards and Technology (NIST)-certified soil standards were spiked with standard solutions, mixed well, desiccated, and analyzed by an energy dispersive XRF. Homogenous targets were produced and low error calibration curves, for the added and not added, neighboring, elements, were obtained. With the addition of few elements, the technique provides reliable multielemental analysis, even for concentrations of the order of milligram per kilogram (ppm). When results were compared to the ones obtained from XRF commercial quantitation software programs, which are widely used in environmental monitoring and assessment applications, they were found to fit certified values better. Moreover, in all examined cases, results were reliable. Hence, this technique can also be used to overcome difficulties associated with interlaboratory consistency and for cross-validating results. The technique was applied to samples with an environmental interest, collected from a ship/boat repainting area. Increased copper, zinc, and lead loads were observed (284, 270, and 688 mg/kg maximum concentrations in soil, respectively), due to vessels being paint stripped and repainted.

  14. [Application of the racial algorithm in energy dispersive X-ray fluorescence overlapped spectrum analysis].

    PubMed

    Zeng, Guo-Qiang; Luo, Yao-Yao; Ge, Liang-Quan; Zhang, Qing-Xian; Gu, Yi; Cheng, Feng

    2014-02-01

    In the energy dispersive X-ray fluorescence spectrum analysis, scintillation detector such as NaI (Tl) detector usually has a low energy resolution at around 8%. The low energy resolution causes problems in spectral data analysis especially in the high background and low counts condition, it is very limited to strip the overlapped spectrum, and the more overlapping the peaks are, the more difficult to peel the peaks, and the qualitative and quantitative analysis can't be carried out because we can't recognize the peak address and peak area. Based on genetic algorithm and immune algorithm, we build a new racial algorithm which uses the Euclidean distance as the judgment of evolution, the maximum relative error as the iterative criterion to be put into overlapped spectrum analysis, then we use the Gaussian function to simulate different overlapping degrees of the spectrum, and the racial algorithm is used in overlapped peak separation and full spectrum simulation, the peak address deviation is in +/- 3 channels, the peak area deviation is no more than 5%, and it is proven that this method has a good effect in energy dispersive X-ray fluorescence overlapped spectrum analysis.

  15. Synchrotron Radiation μ-X Ray Fluorescence on Multicellular Tumor Spheroids

    NASA Astrophysics Data System (ADS)

    Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Monti, F.; Colombatti, M.

    2003-01-01

    Synchrotron Radiation micro X-Ray Fluorescence (SR μ-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

  16. Synchrotron Radiation {mu}-X Ray Fluorescence on Multicellular Tumor Spheroids

    SciTech Connect

    Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Colombatti, M.; Monti, F.

    2003-01-24

    Synchrotron Radiation micro X-Ray Fluorescence (SR {mu}-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

  17. Determination of selenium in biological samples with an energy-dispersive X-ray fluorescence spectrometer.

    PubMed

    Li, Xiaoli; Yu, Zhaoshui

    2016-05-01

    Selenium is both a nutrient and a toxin. Selenium-especially organic selenium-is a core component of human nutrition. Thus, it is very important to measure selenium in biological samples. The limited sensitivity of conventional XRF hampers its widespread use in biological samples. Here, we describe the use of high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-Ray fluorescence spectroscopy (EDXRF) in tandem with a three-dimensional optics design to determine 0.1-5.1μgg(-1) levels of selenium in biological samples. The effects of various experimental parameters such as applied voltage, acquisition time, secondary target and various filters were thoroughly investigated. The detection limit of selenium in biological samples via high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-ray fluorescence spectroscopy was decreased by one order of magnitude versus conventional XRF (Paltridge et al., 2012) and found to be 0.1μg/g. To the best of our knowledge, this is the first report to describe EDXRF measurements of Se in biological samples with important implications for the nutrition and analytical chemistry communities.

  18. Real-Time Studies of Gallium Adsorption and Desorption Kinetics by Grazing-Incidence Small-Angle X-ray Scattering and X-ray Fluorescence

    SciTech Connect

    Wang, Y.; Ozcan, A; Ludwig, K; Bhattacharyya, A

    2008-01-01

    Gallium adsorption and desorption on c-plane sapphire has been studied by real-time grazing incidence small-angle x-ray scattering and x-ray fluorescence as a function of substrate temperature (680-740 C) and Ga flux. The x-ray techniques monitor the surface morphology evolution and amount of Ga on the surface. During deposition, nanodroplets of liquid Ga are observed to form on the surface and coarsen. The growth of droplet size during continuous deposition follows dynamical scaling, in agreement with expectations from theory and simulations which include deposition-induced droplet coalescence. However, observation of continued droplet distance scale coarsening during desorption points to the necessity of including further physical processes in the modeling. The desorption rate at different substrate temperatures gives the activation energy of Ga desorption as 2.7 eV, comparable to measured activation energies for desorption from Ga droplets on other substrates and to the Ga heat of vaporization.

  19. Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups.

    PubMed

    Rauwolf, M; Turyanskaya, A; Roschger, A; Prost, J; Simon, R; Scharf, O; Radtke, M; Schoonjans, T; Guilherme Buzanich, A; Klaushofer, K; Wobrauschek, P; Hofstaetter, J G; Roschger, P; Streli, C

    2017-01-01

    In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-µXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its Kα XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution.

  20. Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups

    PubMed Central

    Rauwolf, M.; Turyanskaya, A.; Roschger, A.; Prost, J.; Simon, R.; Scharf, O.; Radtke, M.; Schoonjans, T.; Guilherme Buzanich, A.; Klaushofer, K.; Wobrauschek, P.; Hofstaetter, J. G.; Roschger, P.; Streli, C.

    2017-01-01

    In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-µXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its Kα XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution. PMID:28009572

  1. X-ray structure refinement using aspherical atomic density functions obtained from quantum-mechanical calculations.

    PubMed

    Jayatilaka, Dylan; Dittrich, Birger

    2008-05-01

    An approach is outlined for X-ray structure refinement using atomic density fragments obtained by Hirshfeld partitioning of quantum-mechanical density fragments. Results are presented for crystal structure refinements of urea and benzene using these 'Hirshfeld atoms'. Using this procedure, the quantum-mechanical non-spherical electron density is taken into account in the structural model based on the conformation found in the crystal. Contrary to current consensus in structure refinement, the anisotropic displacement parameters of H atoms can be reproduced from neutron diffraction measurements simply from a least-squares fit using the Hirshfeld atoms derived from the BLYP level of theory and including a simple point-charge model to treat the crystal environment.

  2. X-ray-photon scattering by an excited and ionized atom

    NASA Astrophysics Data System (ADS)

    Hopersky, Alexey N.; Nadolinsky, Alexey M.; Novikov, Sergey A.; Yavna, Victor A.

    2015-02-01

    The scattering process of an x-ray photon by an excited and ionized many-electron atom with attosecond photon-electron contact interaction is theoretically investigated. The results of the authors' recent work [Hopersky et al., Phys. Rev. A 88, 032704 (2013), 10.1103/PhysRevA.88.032704] are generalized for the cases of (a) arbitrary energy of the photon that prepares the scattering state and (b) the scattering of the photon by the continuous spectrum electron of the ionization state of the atom. The atom of Ne is considered as the object of the study. Along with the effects of normal Compton and elastic scattering, the existence of anomalous inelastic scattering is predicted. It may be assumed that this effect will become a basis for an experimental method of increasing the energy of the photons generated, for example, by a free-electron x-ray laser. It is determined that during the elastic scattering of a photon by an electron of the continuous spectrum, along with the known contribution from the jl Bessel function over the l =0 harmonic (Thomson scattering), there is also a contribution from Bessel functions with harmonics l ∈[1 ;∞ ) . The experimental discovery and application of the anomalous Compton photon scattering effect directly by the atomic electron of the continuous spectrum have their own practical interest.

  3. Determination of fluorine concentrations using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry to analyze fluoride precipitates.

    NASA Astrophysics Data System (ADS)

    Lee, H. A.; Lee, J.; Kwon, E.; Kim, D.; Yoon, H. O.

    2015-12-01

    In recent times, fluorine has been receiving increasing attention due to the possibility for chemical (HF) leakage accidents and its high toxicity to human and environment. In this respect, a novel approach for the determination of fluorine concentrations in water samples using wavelength dispersive X-ray fluorescence (WDXRF) spectrometry was investigated in this study. The main disadvantage of WDXRF technique for fluorine analysis is low analytical sensitivity for light elements with atomic number (Z) less than 15. To overcome this problem, we employed the precipitation reaction which fluoride is reacted with cation such as Al3+ and/or Ca2+ prior to WDXRF analysis because of their high analytical sensitivity. The cation was added in fluoride solutions to form precipitate (AlF3 and/or CaF2) and then the solution was filtered through Whatman filter. After drying at 60 °C for 5 min, the filter was coated with X-ray film and directly analyzed using WDXRF spectrometry. Consequently, we analyzed the cation on filter and subsequently fluorine concentration was calculated inversely based on chemical form of precipitate. This method can improve the analytical sensitivity of WDXRF technique for fluorine analysis and be applicable to various elements that can make precipitate.

  4. The BioCAT Microprobe for X-Ray Fluorescence Imaging, MicroXAFS and Microdiffraction Studies on Biological Samples

    SciTech Connect

    Barrea, R.A.; Gore, D.; Kondrashkina, E.; Weng, T.; Heurich, R.; Vukonich, M.; Orgel, J.; Davidson, M.; Collingwood, J.F.; Mikhaylova, A.; Irving, T.C.

    2007-07-31

    Microbeam capabilities have been recently added to the Biophysics Collaborative Access Team (BioCAT) beamline 18-ID at the Advanced Photon Source to allow x-ray elemental mapping, micro x-ray absorption fine structure and microdiffraction studies on biological samples. The microprobe setup comprises a pair of platinum coated silicon KB mirrors; a sample holder mounted in a high precision positioner (100 nm accuracy); fluorescence detectors including a Si drift detector, Fe and Zn Bent Laue analyzers and a Ge detector; and a CCD detector for micro-diffraction experiments. The energy range of the microprobe is from 3.5 keV up to 17 keV. The fast scanning capabilities of the Bio-CAT beamline facilitate rapid acquisition of x-ray elemental images and micro-XAFS spectra. This paper reports the results of commissioning the KB mirror system and its performance in initial x-ray fluorescence mapping and micro-diffraction studies.

  5. X-ray holographic microscopy using the atomic-force microscope

    SciTech Connect

    Howells, M.R.; Jacobsen, C.J.; Lindaas, S.

    1993-09-01

    The present authors have been seeking for some time to improve the resolution of holographic microscopy and have engaged in a continuing series of experiments using the X1A soft x-ray undulator beam line at Brookhaven. The principle strategy for pushing the resolution lower in these experiments has been the use of polymer resists as x-ray detectors and the primary goal has been to develop the technique to become useful for examining wet biological material. In the present paper the authors report on progress in the use of resist for high-spatial-resolution x-ray detection. This is the key step in in-line holography and the one which sets the ultimate limit to the image resolution. The actual recording has always been quite easy, given a high-brightness undulator source, but the difficult step was the readout of the recorded pattern. The authors describe in what follows how they have built a special instrument: an atomic force microscope (AFM) to read holograms recorded in resist. They report the technical reasons for building, rather than buying, such an instrument and they give details of the design and performance of the device. The authors also describe the first attempts to use the system for real holography and the authors show results of both recorded holograms and the corresponding reconstructed images. Finally, the authors try to analyze the effect that these advances are likely to have on the future prospects for success in applications of x-ray holography and the degree to which the other technical systems that are needed for such success are available or within reach.

  6. Micro-X-Ray Fluorescence Spectrometry of the Surface Elemental Composition of Vegetative Parts and Fruiting Bodies of Lichenized Teloschistaceae Fungi

    NASA Astrophysics Data System (ADS)

    Biazrov, L. G.; Pelgunova, L. A.

    2016-01-01

    The elemental composition and atomic mass ratios (%) on the surface of vegetative and generative parts of crustose Caloplaca cerina and foliose Xanthoria parietina lichen thalli collected from the same tree trunk were measured using micro-x-ray fluorescence spectrometry. The atomic mass fractions for half of the elements (of 21 identified) were significantly higher on the surfaces of fruiting bodies (apothecia) than on vegetative parts of thalli of both species. The atomic mass fractions of most elements were much greater on the surfaces of fruiting bodies and vegetative parts of the foliose species than on the crustose species.

  7. Fiber-optic based in situ atomic spectroscopy for manufacturing of x-ray optics

    NASA Astrophysics Data System (ADS)

    Atanasoff, George; Metting, Christopher J.; von Bredow, Hasso

    2016-09-01

    The manufacturing of multilayer Laue (MLL) components for X-ray optics by physical vapor deposition (PVD) requires high precision and accuracy that presents a significant process control challenge. Currently, no process control system provides the accuracy, long-term stability and broad capability for adoption in the manufacturing of X-ray optics. In situ atomic absorption spectroscopy is a promising process control solution, capable of monitoring the deposition rate and chemical composition of extremely thin metal silicide films during deposition and overcoming many limitations of the traditional methods. A novel in situ PVD process control system for the manufacturing of high-precision thin films, based on combined atomic absorption/emission spectrometry in the vicinity of the deposited substrate, is described. By monitoring the atomic concentration in the plasma region independently from the film growth on the deposited substrate, the method allows deposition control of extremely thin films, compound thin films and complex multilayer structures. It provides deposition rate and film composition measurements that can be further utilized for dynamic feedback process control. The system comprises a reconfigurable hardware module located outside the deposition chamber with hollow cathode light sources and a fiber-optic-based frame installed inside the deposition chamber. Recent experimental results from in situ monitoring of Al and Si thin films deposited by DC and RF magnetron sputtering at a variety of plasma conditions and monitoring configurations are presented. The results validate the operation of the system in the deposition of compound thin films and provide a path forward for use in manufacturing of X-Ray optics.

  8. A wavelength dispersive detector for synchrotron x-ray fluorescence microprobe analysis (abstract)

    NASA Astrophysics Data System (ADS)

    Rivers, Mark L.; Sutton, Stephen R.

    1995-02-01

    The synchrotron x-ray fluorescence (SXRF) microprobe has proven to be a valuable tool for trace element research. It permits analysis down to a few parts per million of many elements in a spot size of less than 10 μm. Existing SXRF microprobes are using energy dispersive detectors (EDS), either Si(Li) or intrinsic Ge diodes. Such detectors have the advantage of collecting the entire fluorescence spectrum at once. They can also be positioned to collect a relatively large solid angle. However, EDS detectors suffer from several significant problems: resolution at Fe Kα is about 150 eV, which is roughly 60 times the natural linewidth; the maximum count rate is less than 20 000 counts/s in the entire spectrum; there is significant low-energy background due to scattering and incomplete charge collection in the device. For geochemical analyses these limitations preclude trace element analyses in the presence of a large amount of a high atomic number element: for example, trace element studies of galena (PbS) and zircon (ZrSiO4), or measurements of Cr or Ti in minerals with more than a few percent Fe or Mn. The poor energy resolution prevents the measurement of small amounts of rare-earth elements in samples with significant concentrations of first-row transition elements. Wavelength dispersive spectrometers, based upon Bragg diffraction from a bent crystal, have several distinct advantages over EDS detectors. The resolution at Fe Kα is about 10 eV, or only 4 times the natural linewidth. This permits the analysis of rare-earth elements and also lowers the background which improves detection limits to the 0.1 ppm range. The WDS spectrometer only detects a single energy at once, so it is possible to measure trace elements in the presence of intense fluorescence of a major element. We have installed a commercial wavelength dispersive spectrometer (model WDX-3PC from Microspec Corp., Fremont, CA) on the X-26A microprobe beamline at the NSLS. The spectrometer can scan the

  9. Minority additive distributions in a ceramic metal-halide arc lamp using high-energy x-ray induced fluorescence

    NASA Astrophysics Data System (ADS)

    Curry, J. J.; Adler, H. G.; Shastri, S. D.; Lawler, J. E.

    2001-09-01

    X-ray induced fluorescence is used to measure the elemental densities of minority additives in a metal-halide arc contained inside a translucent ceramic envelope. A monochromatic x-ray beam from the Sector 1 Insertion Device beamline at the Advanced Photon Source is used to excite K-shell x-ray fluorescence in the constituents of a ceramic metal-halide arc lamp dosed with DyI3 and CsI. Fluorescence and scattered photons are collected by a cryogenic energy-resolving Ge detector. The high signal-to-noise spectra show strong fluorescence from Dy, Cs, and I, as well as elastic scattering from Hg. Radial distributions of the absolute elemental densities of Dy, Cs, and I are obtained.

  10. Minority additive distributions in a ceramic metal-halide arc lamp using high-energy x-ray induced fluorescence

    SciTech Connect

    Curry, J. J.; Adler, H. G.; Shastri, S. D.; Lawler, J. E.

    2001-09-24

    X-ray induced fluorescence is used to measure the elemental densities of minority additives in a metal-halide arc contained inside a translucent ceramic envelope. A monochromatic x-ray beam from the Sector 1 Insertion Device beamline at the Advanced Photon Source is used to excite K-shell x-ray fluorescence in the constituents of a ceramic metal-halide arc lamp dosed with DyI{sub 3} and CsI. Fluorescence and scattered photons are collected by a cryogenic energy-resolving Ge detector. The high signal-to-noise spectra show strong fluorescence from Dy, Cs, and I, as well as elastic scattering from Hg. Radial distributions of the absolute elemental densities of Dy, Cs, and I are obtained.

  11. Atomic motion of resonantly vibrating quartz crystal visualized by time-resolved X-ray diffraction

    SciTech Connect

    Aoyagi, Shinobu; Osawa, Hitoshi; Sugimoto, Kunihisa; Fujiwara, Akihiko

    2015-11-16

    Transient atomic displacements during a resonant thickness-shear vibration of AT-cut α-quartz are revealed by time-resolved X-ray diffraction under an alternating electric field. The lattice strain resonantly amplified by the alternating electric field is ∼10{sup 4} times larger than that induced by a static electric field. The resonantly amplified lattice strain is achieved by fast displacements of oxygen anions and collateral resilient deformation of Si−O−Si angles bridging rigid SiO{sub 4} tetrahedra, which efficiently transduce electric energy into elastic energy.

  12. Excitation and propagation of X-ray fluorescence through thin devices with hollowed ordered structures: comparison of experimental and theoretical spectra.

    PubMed

    Mazuritskiy, M I; Dabagov, S B; Marcelli, A; Lerer, A M; Dziedzic-Kocurek, K

    2016-01-01

    The lack of models describing the propagation of X-rays in waveguides and the interference mechanism between incident and reflected radiation waves hamper the understanding and the control of wave propagation phenomena occurring in many real systems. Here, experimental spectra collected at the exit of microchannel plates (MCPs) under the total X-ray reflection condition are presented. The results are discussed in the framework of a theoretical model in which the wave propagation is enhanced by the presence of a transition layer at the surface. The angular distributions of the propagating radiation at the exit of these MCPs with microchannels of ∼3 µm diameter will also be presented and discussed. These spectra show contributions associated with the reflection of the primary monochromatic beam and with the fluorescence radiation originating from the excitation of atoms composing the surface of the microchannel. The soft X-ray fluorescence spectra collected at the exit of microcapillaries were analyzed in the framework of a wave approximation while diffraction contributions observed at the exit of these hollow X-ray waveguides have been calculated using the Fraunhofer diffraction model for waves in the far-field domain. Data collected at the Si L-edge show that in glassy MCPs the fluorescence radiation can be detected only when the energy of the primary monochromatic radiation is above the absorption edge for grazing angles higher than half of the critical angle of the total reflection phenomenon. Experimental data and simulations of the propagating radiation represent a clear experimental confirmation of the channeling phenomenon of the excited fluorescence radiation inside a medium and point out that a high transmission can be obtained in waveguide optics for parameters relevant to X-ray imaging.

  13. Simulated 'On-Line' Wear Metal Analysis of Lubricating Oils by X-Ray Fluorescence Spectroscopy

    NASA Technical Reports Server (NTRS)

    Kelliher, Warren C.; Partos, Richard D.; Nelson, Irina

    1996-01-01

    The objective of this project was to assess the sensitivity of X-ray Fluorescence Spectroscopy (XFS) for quantitative evaluation of metal particle content in engine oil suspensions and the feasibility of real-time, dynamic wear metal analysis. The study was focused on iron as the majority wear metal component. Variable parameters were: particle size, particle concentration and oil velocity. A commercial XFS spectrometer equipped with interchangeable static/dynamic (flow cell) sample chambers was used. XFS spectra were recorded for solutions of Fe-organometallic standard and for a series of DTE oil suspensions of high purity spherical iron particles of 2g, 4g, and 8g diameter, at concentrations from 5 ppm to 5,000 ppm. Real contaminated oil samples from Langley Air Force Base aircraft engines and NASA Langley Research Center wind tunnels were also analyzed. The experimental data conform the reliability of XFS as the analytical method of choice for this project. Intrinsic inadequacies of the instrument for precise analytic work at low metal concentrations were identified as being related to the particular x-ray beam definition, system geometry, and flow-cell materials selection. This work supports a proposal for the design, construction and testing of a conceptually new, miniature XFS spectrometer with superior performance, dedicated to on-line, real-time monitoring of lubricating oils in operating engines. Innovative design solutions include focalization of the incident x-ray beam, non-metal sample chamber, and miniaturization of the overall assembly. The instrument would contribute to prevention of catastrophic engine failures. A proposal for two-year funding has been presented to NASA Langley Research Center Internal Operation Group (IOG) Management, to continue the effort begun by this summer's project.

  14. Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

    NASA Astrophysics Data System (ADS)

    Nikonow, Wilhelm; Rammlmair, Dieter

    2016-11-01

    Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

  15. Resonant inelastic scattering in dilute magnetic semiconductors by x-ray fluorescence spectroscopy

    SciTech Connect

    Lawniczak-Jablonska, K. |; Jia, J.J.; Underwood, J.H.

    1997-04-01

    As modern, technologically important materials have become more complex, element specific techniques have become invaluable in studying the electronic structure of individual components from the system. Soft x-ray fluorescence (SXF) and absorption (SXA) spectroscopies provide a unique means of measuring element and angular momentum density of electron states, respectively, for the valence and conducting bands in complex materials. X-ray absorption and the decay through x-ray emission are generally assumed to be two independent one-photon processes. Recent studies, however have demonstrated that SXF excited near the absorption threshold generate an array of spectral features that depend on nature of materials, particularly on the localization of excited states in s and d-band solids and that these two processes can no be longer treated as independent. Resonant SXF offers thus the new way to study the dynamics of the distribution of electronic valence states in the presence of a hole which is bound to the electron low lying in the conduction band. This process can simulate the interaction between hole-electron pair in wide gap semiconductors. Therefore such studies can help in understanding of transport and optics phenomena in the wide gap semiconductors. The authors report the result of Mn and S L-resonant emission in Zn{sub 1{minus}x}Mn{sub x}S (with x=0.2 and 0.3) and MnS as the energy of exciting radiation is tuned across the Mn and S L{sub 3,2} absorption edge, along with the resonant excited spectra from elemental Mn as a reference.

  16. Time-Lapse Observation of Electrolysis of Copper Sulfate with a Full-Field X-ray Fluorescence Imaging Microscope

    NASA Astrophysics Data System (ADS)

    Ohigashi, Takuji; Aota, Tatsuya; Watanabe, Norio; Takano, Hidekazu; Yokosuka, Hiroki; Aoki, Sadao

    2008-06-01

    The time-lapse observation of the electrodeposition of copper in copper sulfate solution was performed by imaging X-ray fluorescence from the copper deposition. The X-ray fluorescence was directly imaged with a full-field Wolter mirror microscope, which was constructed at the Photon Factory. Controlling the electric current in the solution from 0 to 71.7 µA, the deposition of copper on a Pt cathode was directly observed by imaging its X-ray fluorescence. One exposure time for obtaining an X-ray fluorescence image was 80 s. Then, it was 17 min later from the beginning of the electrolysis when the X-ray fluorescence image of the electrodeposition is observed for the first time. At this exposure time, the detection limit of the mass of copper was estimated to be 0.60 pg/image, which was calculated using test samples of 1.00×10-3-1.00 mol/l copper sulfate solutions.

  17. Changes in the Atomic Structure through Glass Transition Observed by X-Ray Scattering

    SciTech Connect

    Egami, Takeshi

    2012-01-01

    The glass transition involves a minor change in the internal energy, and yet the physical and mechanical properties of a glass change dramatically. In order to determine the evolution of the atomic structure through the glass transition, we employed in-situ synchrotron X-ray scattering measurements as a function of temperature on a model material: Zr-Cu-Al metallic glass. We found that the thermal expansion at the atomic level is smaller than the macroscopic thermal expansion, and significantly increases above the glass transition temperature. The observed changes in the pair-distribution function (PDF) are explained in terms of the fluctuations in the local atomic volume and their change through the glass transition.

  18. Electrochemical X-ray fluorescence spectroscopy for trace heavy metal analysis: enhancing X-ray fluorescence detection capabilities by four orders of magnitude.

    PubMed

    Hutton, Laura A; O'Neil, Glen D; Read, Tania L; Ayres, Zoë J; Newton, Mark E; Macpherson, Julie V

    2014-05-06

    The development of a novel analytical technique, electrochemical X-ray fluorescence (EC-XRF), is described and applied to the quantitative detection of heavy metals in solution, achieving sub-ppb limits of detection (LOD). In EC-XRF, electrochemical preconcentration of a species of interest onto the target electrode is achieved here by cathodic electrodeposition. Unambiguous elemental identification and quantification of metal concentration is then made using XRF. This simple electrochemical preconcentration step improves the LOD of energy dispersive XRF by over 4 orders of magnitude (for similar sample preparation time scales). Large area free-standing boron doped diamond grown using microwave plasma chemical vapor deposition techniques is found to be ideal as the electrode material for both electrodeposition and XRF due to its wide solvent window, transparency to the XRF beam, and ability to be produced in mechanically robust freestanding thin film form. During electrodeposition it is possible to vary both the deposition potential (Edep) and deposition time (tdep). For the metals Cu(2+) and Pb(2+) the highest detection sensitivities were found for Edep = -1.75 V and tdep (=) 4000 s with LODs of 0.05 and 0.04 ppb achieved, respectively. In mixed Cu(2+)/Pb(2+) solutions, EC-XRF shows that Cu(2+) deposition is unimpeded by Pb(2+), across a broad concentration range, but this is only true for Pb(2+) when both metals are present at low concentrations (10 nM), boding well for trace level measurements. In a dual mixed metal solution, EC-XRF can also be employed to either selectively deposit the metal which has the most positive formal reduction potential, E(0), or exhaustively deplete it from solution, enabling uninhibited detection of the metal with the more negative E(0).

  19. An Atomic-Scale X-ray View of Functional Oxide Films

    NASA Astrophysics Data System (ADS)

    Tung, I.-Cheng

    Complex oxides are a class of materials that exhibit a wide variety of physical functionalities, such as ferroelectricity, colossal magnetoresistance, mulitferroicity and superconductivity, with outstanding potential for meeting many of our technological demands. The primary objective of this dissertation is to understand the structural and electronic behavior of complex oxide ultrathin films subjected to confinement, lattice misfit and broken symmetry at the interface. In complex oxide ultrathin films, heteroepitaxial synthesis has evolved into a reliable strategy to engineer orbital-lattice interactions in correlated materials and led to new and entirely unexpected phenomena at their interfaces. I experimentally demonstrated that the bulk crystal symmetry directs the atomic and orbital responses adopted by coherently strained ultrathin films of RNiO3 (R = La, Nd) with detailed X-ray scattering, polarization-dependent X-ray absorption spectroscopy (XAS) and supported by a mathematical point group symmetry analysis, found that strain-stabilized phases maintain a ``memory'' of their bulk state. This topic, however, touched only upon the properties of such films. A fundamental challenge in this research area occurs before this and centers around the understanding of how to create high-quality films with arbitrary configurations. A longstanding challenge in the oxide thin film community has been the growth of An+1BnO3 n+1 Ruddlesden-Popper (RP) compounds. To understand this problem, we have utilized a newly constructed oxide MBE with in situ synchrotron X-ray scattering capability to study the initial growth of such layered oxides and track the dynamic evolution. X-ray results are supported by theoretical calculations that demonstrated the layered oxide films dynamically rearrange during growth, leading to structures that are highly unexpected, and suggest a general approach that may be essential for the construction of metastable RP phases with performing the first

  20. Detection of Fingerprints Based on Elemental Composition Using Micro-X-Ray Fluorescence.

    SciTech Connect

    Worley, C. G.; Wiltshire, S.; Miller, T. C.; Havrilla, G. J.; Majidi, V.

    2005-01-01

    A method was developed to detect fingerprints using a technique known as micro-X-ray fluorescence. The traditional method of detecting fingerprints involves treating the sample with certain powders, liquids, or vapors to add color to the fingerprint so that it can be easily seen and photographed for forensic purposes. This is known as contrast enhancement, and a multitude of chemical processing methods have been developed in the past century to render fingerprints visible. However, fingerprints present on certain substances such as fibrous papers and textiles, wood, leather, plastic, adhesives, and human skin can sometimes be difficult to detect by contrast enhancement. Children's fingerprints are also difficult to detect due to the absence of sebum on their skin, and detection of prints left on certain colored backgrounds can sometimes be problematic. Micro-X-ray fluorescence (MXRF) was studied here as a method to detect fingerprints based on chemical elements present in fingerprint residue. For example, salts such as sodium chloride and potassium chloride excreted in sweat are sometimes present in detectable quantities in fingerprints. We demonstrated that MXRF can be used to detect this sodium, potassium, and chlorine from such salts. Furthermore, using MXRF, each of these elements (and many other elements if present) can be detected as a function of location on a surface, so we were able to 'see' a fingerprint because these salts are deposited mainly along the patterns present in a fingerprint (traditionally called friction ridges in forensic science). MXRF is not a panacea for detecting all fingerprints; some prints will not contain enough detectable material to be 'seen'; however, determining an effective means of coloring a fingerprint with traditional contrast enhancement methods can sometimes be an arduous process with limited success. Thus, MXRF offers a possible alternative for detecting fingerprints, and it does not require any additional chemical

  1. Imaging metals in proteins by combining electrophoresis with rapid x-ray fluorescence mapping.

    SciTech Connect

    Finney, L.; Chishti, Y.; Khare, T.; Giometti, C.; Levina, A.; Lay, P. A.; Vogt, S.; Univ. of Sydney; Northwestern Univ.

    2010-01-01

    Growing evidence points toward a very dynamic role for metals in biology. This suggests that physiological circumstance may mandate metal ion redistribution among ligands. This work addresses a critical need for technology that detects, identifies, and measures the metal-containing components of complex biological matrixes. We describe a direct, user-friendly approach for identifying and quantifying metal?protein adducts in complex samples using native- or SDS-PAGE, blotting, and rapid synchrotron X-ray fluorescence mapping with micro-XANES (X-ray absorption near-edge structure) of entire blots. The identification and quantification of each metal bound to a protein spot has been demonstrated, and the technique has been applied in two exemplary cases. In the first, the speciation of the in vitro binding of exogenous chromium to blood serum proteins was influenced markedly by both the oxidation state of chromium exposed to the serum proteins and the treatment conditions, which is of relevance to the biochemistry of Cr dietary supplements. In the second case, in vivo changes in endogenous metal speciation were examined to probe the influence of oxygen depletion on iron speciation in Shewanella oneidensis.

  2. Total reflection X-ray fluorescence (TXRF) for direct analysis of aerosol particle samples.

    PubMed

    Bontempi, E; Zacco, A; Benedetti, D; Borgese, L; Colombi, P; Stosnach, H; Finzi, G; Apostoli, P; Buttini, P; Depero, L E

    2010-04-14

    Atmospheric aerosol particles have a great impact on the environment and on human health. Routine analysis of the particles usually involves only the mass determination. However, chemical composition and phases provide fundamental information about the particles' origins and can help to prevent health risks. For example, these particles may contain heavy metals such as Pb, Ni and Cd, which can adversely affect human health. In this work, filter samples were collected in Brescia, an industrial town located in Northern Italy. In order to identify the chemical composition and the phases of the atmospheric aerosols, the samples were analysed by means of total reflection X-ray fluorescence (TXRF) spectrometry with a laboratory instrument and X-ray microdiffraction at Synchrotron Daresbury Laboratories, Warrington (Cheshire, UK). The results are discussed and correlated to identify possible pollution sources. The novelty of this analytical approach is that filter samples for TXRF were analysed directly and did not require chemical pretreatment to leach elements from the aerosol particulates. The results of this study clearly show that TXRF is a powerful technique for the analysis of atmospheric aerosols on 'as-received' filters, thereby leaving samples intact and unaltered for possible subsequent analyses by other methods. In addition, the low detection limits for many elements (low ng/cm2) indicate that this method may hold promise in various application fields, such as nanotechnology.

  3. Deformulation of a solid pharmaceutical form using computed tomography and X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Oliveira Junior, J. M.; Balcão, V. M.; Vila, M. M. D. C.; Aranha, N.; Yoshida, V. M. H.; Chaud, M. V.; Mangine Filho, S.

    2015-07-01

    Deformulation of medicines is of undeniable importance, since it can be utilized both to unravel the chemical composition of the excipients integrating a pharmaceutical formulation of a specific medicine and as an important tool to conduct morphometric studies of the formulation under study. Such strategy may be utilized in analytical studies aiming at quantifying the components of reference drugs, or in the identification of putative counterfeit pharmaceuticals. Deformulation makes use of physicochemical analysis tools to characterize, from the chemical point of view, the components integrating medicine pharmaceutical formulations and from the physical point of view, the morphological part of the pharmaceutical formulation. The techniques of computer tomography (SkyScan 1174 - Bruker microCT) and X-ray fluorescence analyses (using an X-ray source with W-anode from Hammatsu Photonics and Silicon Drift detector from Amptek) were successfully used in performing a process of deformulation of a solid pharmaceutical formulation of tablets, utilized herein as a model medicine for controlled drug release. The analytical methods used in this work, proved their effectiveness for the main goal of this study, which aimed to characterize a pharmaceutical formulation via its deconstruction.

  4. Spectrum reconstruction method based on the detector response model calibrated by x-ray fluorescence.

    PubMed

    Li, Ruizhe; Li, Liang; Chen, Zhiqiang

    2017-02-07

    Accurate estimation of distortion-free spectra is important but difficult in various applications, especially for spectral computed tomography. Two key problems must be solved to reconstruct the incident spectrum. One is the acquisition of the detector energy response. It can be calculated by Monte Carlo simulation, which requires detailed modeling of the detector system and a high computational power. It can also be acquired by establishing a parametric response model and be calibrated using monochromatic x-ray sources, such as synchrotron sources or radioactive isotopes. However, these monochromatic sources are difficult to obtain. Inspired by x-ray fluorescence (XRF) spectrum modeling, we propose a feasible method to obtain the detector energy response based on an optimized parametric model for CdZnTe or CdTe detectors. The other key problem is the reconstruction of the incident spectrum with the detector response. Directly obtaining an accurate solution from noisy data is difficult because the reconstruction problem is severely ill-posed. Different from the existing spectrum stripping method, a maximum likelihood-expectation maximization iterative algorithm is developed based on the Poisson noise model of the system. Simulation and experiment results show that our method is effective for spectrum reconstruction and markedly increases the accuracy of XRF spectra compared with the spectrum stripping method. The applicability of the proposed method is discussed, and promising results are presented.

  5. Spectrum reconstruction method based on the detector response model calibrated by x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Li, Ruizhe; Li, Liang; Chen, Zhiqiang

    2017-02-01

    Accurate estimation of distortion-free spectra is important but difficult in various applications, especially for spectral computed tomography. Two key problems must be solved to reconstruct the incident spectrum. One is the acquisition of the detector energy response. It can be calculated by Monte Carlo simulation, which requires detailed modeling of the detector system and a high computational power. It can also be acquired by establishing a parametric response model and be calibrated using monochromatic x-ray sources, such as synchrotron sources or radioactive isotopes. However, these monochromatic sources are difficult to obtain. Inspired by x-ray fluorescence (XRF) spectrum modeling, we propose a feasible method to obtain the detector energy response based on an optimized parametric model for CdZnTe or CdTe detectors. The other key problem is the reconstruction of the incident spectrum with the detector response. Directly obtaining an accurate solution from noisy data is difficult because the reconstruction problem is severely ill-posed. Different from the existing spectrum stripping method, a maximum likelihood-expectation maximization iterative algorithm is developed based on the Poisson noise model of the system. Simulation and experiment results show that our method is effective for spectrum reconstruction and markedly increases the accuracy of XRF spectra compared with the spectrum stripping method. The applicability of the proposed method is discussed, and promising results are presented.

  6. Modeling of x-ray fluorescence using MCNPX and Geant4

    SciTech Connect

    Rajasingam, Akshayan; Hoover, Andrew S; Fensin, Michael L; Tobin, Stephen J

    2009-01-01

    X-Ray Fluorescence (XRF) is one of thirteen non-destructive assay techniques being researched for the purpose of quantifying the Pu mass in used fuel assemblies. The modeling portion of this research will be conducted with the MCNPX transport code. The research presented here was undertaken to test the capability of MCNPX so that it can be used to benchmark measurements made at the ORNL and to give confidence in the application of MCNPX as a predictive tool of the expected capability of XRF in the context of used fuel assemblies. The main focus of this paper is a code-to-code comparison between MCNPX and Geant4 code. Since XRF in used fuel is driven by photon emission and beta decay of fission fragments, both terms were independently researched. Simple cases and used fuel cases were modeled for both source terms. In order to prepare for benchmarking to experiments, it was necessary to determine the relative significance of the various fission fragments for producing X-rays.

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

    NASA Astrophysics Data System (ADS)

    Óvári, M.; Streli, C.; Wobrauschek, P.; Záray, Gy.

    2009-08-01

    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. Analysis of Russian kopecks (1877-1933) using x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Cavness, B.; Williams, S.

    2013-04-01

    We have analyzed five Russian kopecks minted between the years of 1877 and 1933 using X-ray fluorescence (XRF) as part of an undergraduate research project. The intensities of the Cu K-shell X-rays were studied in order to compare the relative purities of the Cu used to mint the kopecks. The economic conditions under which the kopecks were minted are discussed, as well as impurities discovered during XRF analysis. In addition to XRF analysis, kopecks produced just before (1915) and after (1924) the October Revolution of 1917 were weighed in order to determine whether or not the Decree of February 22, 1924 was carried out. The legislation (enacted by the Central Executive Committee and the Council of the People's Commissaries) decreed that the proportions of pure Ag and Cu used in the minting of new coins should be the identical to those produced before the revolution and that the diameters and weights of the kopecks should also remain the same. The data from our experiments suggest that the legislation was successfully carried out.

  9. In vivo monitoring of toxic metals: assessment of neutron activation and x-ray fluorescence techniques

    SciTech Connect

    Ellis, K.J.

    1986-01-01

    To date, cadmium, lead, aluminum, and mercury have been measured in vivo in humans. The possibilities of monitoring other toxic metals have also been demonstrated, but no human studies have been performed. Neutron activation analysis appears to be most suitable for Cd and Al measurements, while x-ray fluorescence is ideally suited for measurement of lead in superficial bone. Filtered neutron beams and polarized x-ray sources are being developed which will improve in vivo detection limits. Even so, several of the current facilities are already suitable for use in epidemiological studies of selected populations with suspected long-term low-level ''environmental'' exposures. Evaluation and diagnosis of patients presenting with general clinical symptoms attributable to possible toxic metal exposure may be assisted by in vivo examination. Continued in vivo monitoring of industrial workers, especially follow-up measurements, will provide the first direct assessment of changes in body burden and a direct measure of the biological life-times of these metals in humans. 50 refs., 4 figs., 2 tabs.

  10. Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

    PubMed

    Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

    2016-03-15

    A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles.

  11. Investigation of X-ray fluorescence computed tomography (XFCT) and K-edge imaging.

    PubMed

    Bazalova, Magdalena; Kuang, Yu; Pratx, Guillem; Xing, Lei

    2012-08-01

    This work provides a comprehensive Monte Carlo study of X-ray fluorescence computed tomography (XFCT) and K-edge imaging system, including the system design, the influence of various imaging components, the sensitivity and resolution under various conditions. We modified the widely used EGSnrc/DOSXYZnrc code to simulate XFCT images of two acrylic phantoms loaded with various concentrations of gold nanoparticles and Cisplatin for a number of XFCT geometries. In particular, reconstructed signal as a function of the width of the detector ring, its angular coverage and energy resolution were studied. We found that XFCT imaging sensitivity of the modeled systems consisting of a conventional X-ray tube and a full 2-cm-wide energy-resolving detector ring was 0.061% and 0.042% for gold nanoparticles and Cisplatin, respectively, for a dose of ∼ 10 cGy. Contrast-to-noise ratio (CNR) of XFCT images of the simulated acrylic phantoms was higher than that of transmission K-edge images for contrast concentrations below 0.4%.

  12. A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline.

    PubMed

    Fittschen, U; Guilherme, A; Böttger, S; Rosenberg, D; Menzel, M; Jansen, W; Busker, M; Gotlib, Z P; Radtke, M; Riesemeier, H; Wobrauschek, P; Streli, C

    2016-05-01

    An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml(-1) to µg ml(-1)). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml(-1)) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state.

  13. Ground state potential energy surfaces around selected atoms from resonant inelastic x-ray scattering

    NASA Astrophysics Data System (ADS)

    Schreck, Simon; Pietzsch, Annette; Kennedy, Brian; Såthe, Conny; Miedema, Piter S.; Techert, Simone; Strocov, Vladimir N.; Schmitt, Thorsten; Hennies, Franz; Rubensson, Jan-Erik; Föhlisch, Alexander

    2016-01-01

    Thermally driven chemistry as well as materials’ functionality are determined by the potential energy surface of a systems electronic ground state. This makes the potential energy surface a central and powerful concept in physics, chemistry and materials science. However, direct experimental access to the potential energy surface locally around atomic centers and to its long-range structure are lacking. Here we demonstrate how sub-natural linewidth resonant inelastic soft x-ray scattering at vibrational resolution is utilized to determine ground state potential energy surfaces locally and detect long-range changes of the potentials that are driven by local modifications. We show how the general concept is applicable not only to small isolated molecules such as O2 but also to strongly interacting systems such as the hydrogen bond network in liquid water. The weak perturbation to the potential energy surface through hydrogen bonding is observed as a trend towards softening of the ground state potential around the coordinating atom. The instrumental developments in high resolution resonant inelastic soft x-ray scattering are currently accelerating and will enable broad application of the presented approach. With this multidimensional potential energy surfaces that characterize collective phenomena such as (bio)molecular function or high-temperature superconductivity will become accessible in near future.

  14. Ground state potential energy surfaces around selected atoms from resonant inelastic x-ray scattering.

    PubMed

    Schreck, Simon; Pietzsch, Annette; Kennedy, Brian; Såthe, Conny; Miedema, Piter S; Techert, Simone; Strocov, Vladimir N; Schmitt, Thorsten; Hennies, Franz; Rubensson, Jan-Erik; Föhlisch, Alexander

    2016-01-29

    Thermally driven chemistry as well as materials' functionality are determined by the potential energy surface of a systems electronic ground state. This makes the potential energy surface a central and powerful concept in physics, chemistry and materials science. However, direct experimental access to the potential energy surface locally around atomic centers and to its long-range structure are lacking. Here we demonstrate how sub-natural linewidth resonant inelastic soft x-ray scattering at vibrational resolution is utilized to determine ground state potential energy surfaces locally and detect long-range changes of the potentials that are driven by local modifications. We show how the general concept is applicable not only to small isolated molecules such as O2 but also to strongly interacting systems such as the hydrogen bond network in liquid water. The weak perturbation to the potential energy surface through hydrogen bonding is observed as a trend towards softening of the ground state potential around the coordinating atom. The instrumental developments in high resolution resonant inelastic soft x-ray scattering are currently accelerating and will enable broad application of the presented approach. With this multidimensional potential energy surfaces that characterize collective phenomena such as (bio)molecular function or high-temperature superconductivity will become accessible in near future.

  15. Resonance-mediated atomic ionization dynamics induced by ultraintense x-ray pulses

    SciTech Connect

    Ho, Phay J.; Kanter, E. P.; Young, L.

    2015-12-31

    We describe the methodology of our recently developed Monte Carlo rate equation (MCRE) approach, which systematically incorporates bound-bound resonances to model multiphoton ionization dynamics induced by high-fluence, high-intensity x-ray free-electron laser (XFEL) pulses. These resonances are responsible for ionization far beyond that predicted by the sequential single photon absorption model and are central to a quantitative understanding of atomic ionization dynamics in XFEL pulses. We also present calculated multiphoton ionization dynamics for Kr and Xe atoms in XFEL pulses for a variety of conditions, to compare the effects of bandwidth, pulse duration, pulse fluence, and photon energy. This comprehensive computational investigation reveals areas in the photon energy–pulse fluence landscape where resonances are critically important. We also uncover a mechanism, preservation of inner-shell vacancies (PIVS), whereby radiation damage is enhanced at higher XFEL intensities and identify the sequence of core-outer–Rydberg, core-valence, and core-core resonances encountered during multiphoton x-ray ionization.

  16. Ground state potential energy surfaces around selected atoms from resonant inelastic x-ray scattering

    PubMed Central

    Schreck, Simon; Pietzsch, Annette; Kennedy, Brian; Såthe, Conny; Miedema, Piter S.; Techert, Simone; Strocov, Vladimir N.; Schmitt, Thorsten; Hennies, Franz; Rubensson, Jan-Erik; Föhlisch, Alexander

    2016-01-01

    Thermally driven chemistry as well as materials’ functionality are determined by the potential energy surface of a systems electronic ground state. This makes the potential energy surface a central and powerful concept in physics, chemistry and materials science. However, direct experimental access to the potential energy surface locally around atomic centers and to its long-range structure are lacking. Here we demonstrate how sub-natural linewidth resonant inelastic soft x-ray scattering at vibrational resolution is utilized to determine ground state potential energy surfaces locally and detect long-range changes of the potentials that are driven by local modifications. We show how the general concept is applicable not only to small isolated molecules such as O2 but also to strongly interacting systems such as the hydrogen bond network in liquid water. The weak perturbation to the potential energy surface through hydrogen bonding is observed as a trend towards softening of the ground state potential around the coordinating atom. The instrumental developments in high resolution resonant inelastic soft x-ray scattering are currently accelerating and will enable broad application of the presented approach. With this multidimensional potential energy surfaces that characterize collective phenomena such as (bio)molecular function or high-temperature superconductivity will become accessible in near future. PMID:26821751

  17. Preliminary testing of a prototype portable x-ray fluorescence spectrometer. Information circular

    SciTech Connect

    Patten, L.L.; Anderson, N.B.; Stevenson, J.J.

    1982-08-01

    The Federal Bureau of Mines participated with the National Aeronautics and Space Administration and Martin Marietta Aerospace in developing, building, and testing a portable X-ray fluorescence spectrometer for use as an analyzer in mineral-resource investigative work. The prototype battery-powered spectrometer, measuring 11 by 12 by 5 inches and weighing only about 15 pounds, was designed specifically for field use. The spectrometer has two gas-proportional counters and two radioactive sources, (109)Cd and (55)Fe. Preliminary field and laboratory tests on rock specimens and rock pulps have demonstrated the capability of the spectrometer to detect 33 elements, to date. Characteristics of the system present some limitations, however, and further improvements are recommended.

  18. X-Ray Fluorescence to Determine Zn in Bolivian Children using Hair Samples

    SciTech Connect

    Tellería Narvaez, C.A.; Fernández Alcázar, S.; Barrientos Zamora, F.G.; Chungara Castro, J.; Luna Lauracia, I.; Mamani Tola, H.; Mita Peralta, E.; Muñoz Gosálvez, A.O.; Romero Bolaños, L.E.; Ramírez Ávila, G.M.

    2014-06-15

    As a first step in the evaluation of nutritional levels in Bolivian children (8–13 years-old), we carried out X-Ray Fluorescence measurements in hair samples of children belonging to different social classes and living either in rural areas or in cities. The aim of this study is to contribute to health policies tending to improve the global health of children and consequently avoid malnutrition. Our method intends to have maximum reliability and at the same time be as simple as possible from an experimental point of view. Additionally, we use this method to determine some other elements such as Fe, Cu, Pb, As and Hg, the latter three considered as contaminants that could be present in children living in areas which neighbor mines and industries. This work will be complemented by some biological and medical tests.

  19. Elemental Analysis of Variably Contaminated Cremains Using X-ray Fluorescence Spectrometry.

    PubMed

    Gilpin, Megan; Christensen, Angi M

    2015-07-01

    Analyzing and identifying skeletal remains becomes increasingly difficult when remains have been cremated, especially in cases where the cremated material may have been intentionally contaminated with nonskeletal material. This study examined the potential of X-ray fluorescence spectrometry (XRF) to detect the presence of nonskeletal contaminants in samples of cremains. Eleven samples of cremains were variably combined with concrete mix and analyzed using XRF. Photon counts of elements in each sample were analyzed, and the coefficient of determination (R(2)) using unweighted linear regression as a function of percent cremains was calculated. Results showed that with changes in the proportion of skeletal material and contaminant, there were significant (R(2) > 0.90) changes in detected levels of phosphorus, potassium, zinc, aluminum, and sulfur. The use of XRF is concluded to be a valid approach in the identification of the presence of nonskeletal material in potentially contaminated cremains.

  20. 100-OL-1 Operable Unit Field Portable X-Ray Fluorescence (XRF) Analyzer Pilot Study Plans

    SciTech Connect

    Bunn, Amoret L.; Fritz, Brad G.; Wellman, Dawn M.

    2014-07-01

    A pilot study is being conducted to support the approval of the Remedial Investigation/Feasibility Study (RI/FS) Work Plan to evaluate the 100-OL-1 Operable Unit (OU) pre-Hanford orchard lands. Based on comments received by the U.S. Environmental Protection Agency (EPA) and Washington State Department of Ecology, the pilot study will evaluate the use of field portable X-ray fluorescence (XRF) spectrometry measurements for evaluating lead and arsenic concentrations on the soil surface as an indicator of past use of lead arsenate pesticide residue in the OU. The work will be performed in the field during the summer of 2014, and assist in the planning for the characterization activities in the RI/FS.

  1. Development of a combined portable x-ray fluorescence and Raman spectrometer for in situ analysis.

    PubMed

    Guerra, M; Longelin, S; Pessanha, S; Manso, M; Carvalho, M L

    2014-06-01

    In this work, we have built a portable X-ray fluorescence (XRF) spectrometer in a planar configuration coupled to a Raman head and a digital optical microscope, for in situ analysis. Several geometries for the XRF apparatus and digital microscope are possible in order to overcome spatial constraints and provide better measurement conditions. With this combined spectrometer, we are now able to perform XRF and Raman measurements in the same point without the need for sample collection, which can be crucial when dealing with cultural heritage objects, as well as forensic analysis. We show the capabilities of the spectrometer by measuring several standard reference materials, as well as other samples usually encountered in cultural heritage, geological, as well as biomedical studies.

  2. Possible use of pattern recognition for the analysis of Mars rover X-ray fluorescence spectra

    NASA Technical Reports Server (NTRS)

    Yin, Lo I; Trombka, Jacob I.; Seltzer, Stephen M.; Johnson, Robert G.; Philpotts, John A.

    1989-01-01

    On the Mars rover sample-return mission, the rover vehicle will collect and select samples from different locations on the Martian surface to be brought back to earth for laboratory studies. It is anticipated that an in situ energy-dispersive X-ray fluorescence (XRF) spectrometer will be on board the rover. On such a mission, sample selection is of higher priority than in situ quantitative chemical anlaysis. With this in mind, a pattern recognition technique is proposed as a simple, direct, and speedy alternative to detailed chemical analysis of the XRF spectra. The validity and efficacy of the pattern recognition technique are demonstrated by the analyses of laboratory XRF spectra obtained from a series of geological samples, in the form both of standardized pressed pellets and as unprepared rocks. It is found that pattern recognition techniques applied to the raw XRF spectra can provide for the same discrimination among samples as a knowledge of their actual chemical composition.

  3. [Analysis of 14 elements for Jinhua bergamot by X-ray fluorescence spectrometry and elemental analyser].

    PubMed

    Wang, Zhi-gang; Yu, Hong-mei

    2012-01-01

    The content of the elements C, H, O and N in Jinhua bergamot was analysed by using Vario III elemental analyser, the bergamot sample was scanned by using X-ray fluorescence spectrometer with PW2400 wavelength dispersion, and the content of the elements Mg, Al, P, S, Cl, K, Ca, Mn, Fe and Sr was analysed by using IQ+ analytical method. It turned out that the result is more ideal if the content of the elements C, H, O and N is processed as fix phase, and the analytical result is more ideal if, to prevent the sample skin from coming off, the sample is wrapped with mylar film with the film coefficient adjusted.

  4. Petrographic, mineralogic, and x-ray fluorescence analysis of lunar igneous-type rocks and spherules.

    PubMed

    Brown, G M; Emeleus, C H; Holland, J G; Phillips, R

    1970-01-30

    Three lunar rocks show almost identical mineralogy but grain sizes that vary from basaltic to gabbroic. Clinopyroxene is zoned from augite to subcalcic ferroaugite compositions and is accompanied by decrease in Cr, Al, and Ti. Plagioclase is zoned from 93 to 78 percent anorthite. Olivine (68 percent forsterite) is present in one rock and apatite is rare. Cristobalite, ilmenite with Ti-rich lamellae, ulvöspinel (often Cr-rich), troilite, and kamacite are low in trace elements. Glassy spherules are of basaltic or feldspathic (92 percent anorthite) composition but contain abundant iron spheres of taenite composition (13 percent Ni). Four rock analyses by x-ray fluorescence show affinity with terrestrial basalts but with anomalous amounts of Ti, Na, Cr, Zr, Y, Rb, Nb, Ni, Cu, and Zn.

  5. Portable X-ray Fluorescence Spectrometry for the analyses of Cultural Heritage

    NASA Astrophysics Data System (ADS)

    Ridolfi, S.

    2012-07-01

    Field Portable Energy Dispersive X Ray Fluorescence (FP-EDXRF) is particularly useful to analyze works of art, mainly because of his noninvasive and multielemental capability. In many situations FP-EDXRF is the only non invasive technique that can be realistically used to gain some information about the chemical composition of precious and unique objects. Many kind of works, such as paintings, bronzes, precious metals alloys, inks, stones, stamps and more can be studied using a field portable EDXRF system. This manuscript highlights some drawbacks that have to be kept in mind to fulfill a valid measurement such as the need for other backup methods to support portable XRF results or the problem of the non-homogeneity of the sample. This manuscript will also present three examples to demonstrate the usefulness of FP-EDXRF with paintings on canvas, ancient bronzes and sulfur surface analyses.

  6. X-ray spectra of Hercules X-1. 1: Iron line fluorescence from a subrelativistic shell

    NASA Technical Reports Server (NTRS)

    Pravdo, S. H.; Becker, R. H.; Boldt, E. A.; Holt, S. S.; Serlemitsos, P. J.; Swank, J. H.

    1977-01-01

    The X-ray spectrum of Hercules X-1 was observed in the energy range 2-24 keV from August 29 to September 3, 1975. A broad iron line feature is observed in the normal high state spectrum. The line equivalent width is given along with its full-width-half-maximum energy. Iron line fluorescence from an opaque, cool shell of material at the Alfven surface provides the necessary luminosity in this feature. The line energy width can be due to Doppler broadening if the shell is forced to corotate with the pulsar at a radius 800 million cm. Implications of this model regarding physical conditions near Her X-1 are discussed.

  7. Mapping metals in Parkinson's and normal brain using rapid-scanning x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Popescu, Bogdan F. Gh; George, Martin J.; Bergmann, Uwe; Garachtchenko, Alex V.; Kelly, Michael E.; McCrea, Richard P. E.; Lüning, Katharina; Devon, Richard M.; George, Graham N.; Hanson, Akela D.; Harder, Sheri M.; Chapman, L. Dean; Pickering, Ingrid J.; Nichol, Helen

    2009-02-01

    Rapid-scanning x-ray fluorescence (RS-XRF) is a synchrotron technology that maps multiple metals in tissues by employing unique hardware and software to increase scanning speed. RS-XRF was validated by mapping and quantifying iron, zinc and copper in brain slices from Parkinson's disease (PD) and unaffected subjects. Regions and structures in the brain were readily identified by their metal complement and each metal had a unique distribution. Many zinc-rich brain regions were low in iron and vice versa. The location and amount of iron in brain regions known to be affected in PD agreed with analyses using other methods. Sample preparation is simple and standard formalin-fixed autopsy slices are suitable. RS-XRF can simultaneously and non-destructively map and quantify multiple metals and holds great promise to reveal metal pathologies associated with PD and other neurodegenerative diseases as well as diseases of metal metabolism.

  8. Evaluation on determination of iodine in coal by energy dispersive X-ray fluorescence

    USGS Publications Warehouse

    Wang, B.; Jackson, J.C.; Palmer, C.; Zheng, B.; Finkelman, R.B.

    2005-01-01

    A quick and inexpensive method of relative high iodine determination from coal samples was evaluated. Energy dispersive X-ray fluorescence (EDXRF) provided a detection limit of about 14 ppm (3 times of standard deviations of the blank sample), without any complex sample preparation. An analytical relative standard deviation of 16% was readily attainable for coal samples. Under optimum conditions, coal samples with iodine concentrations higher than 5 ppm can be determined using this EDXRF method. For the time being, due to the general iodine concentrations of coal samples lower than 5 ppm, except for some high iodine content coal, this method can not effectively been used for iodine determination. More work needed to meet the requirement of determination of iodine from coal samples for this method. Copyright ?? 2005 by The Geochemical Society of Japan.

  9. Determination of thorium in geological materials by x-ray fluorescence spectrometry after anion exchange extraction

    SciTech Connect

    Roelandts, I.

    1983-08-01

    The exchange capacity of the resin was determined to be 1 m equiv of Th/g dry resin. Synthetic calibration standards of thorium were prepared over a large concentration range, for use as an independent method of calibration. The advantages and disadvantages of direct x-ray fluorescence analysis are discussed. The lower limit of detection has been calculated according to Currie's convention and was found to be equal to 13 ..mu..g of Th/250 mg of resin, sufficient for the range of concentrations found in Th bearing minerals and ores. Results using Canadian syenite rocks and a suite of South African reference minerals show that the proposed method appears to be relatively precise and accurate for exploration geochemistry. 1 figure, 2 tables.

  10. Development of a combined portable x-ray fluorescence and Raman spectrometer for in situ analysis

    NASA Astrophysics Data System (ADS)

    Guerra, M.; Longelin, S.; Pessanha, S.; Manso, M.; Carvalho, M. L.

    2014-06-01

    In this work, we have built a portable X-ray fluorescence (XRF) spectrometer in a planar configuration coupled to a Raman head and a digital optical microscope, for in situ analysis. Several geometries for the XRF apparatus and digital microscope are possible in order to overcome spatial constraints and provide better measurement conditions. With this combined spectrometer, we are now able to perform XRF and Raman measurements in the same point without the need for sample collection, which can be crucial when dealing with cultural heritage objects, as well as forensic analysis. We show the capabilities of the spectrometer by measuring several standard reference materials, as well as other samples usually encountered in cultural heritage, geological, as well as biomedical studies.

  11. X-ray spectra of Hercules X-1. I - Iron line fluorescence from a subrelativistic shell

    NASA Technical Reports Server (NTRS)

    Pravdo, S. H.; Becker, R. H.; Boldt, E. A.; Holt, S. S.; Serlemitsos, P. J.; Swank, J. H.

    1977-01-01

    The X-ray spectrum of Her X-1 was observed in the energy range from 2 to 24 keV from August 29 to September 3, 1975. Emission features are observed near the K-alpha iron-line energy which exhibit both broadening and a double line structure. The total luminosity in these features is about 4 by 10 to the 35th power ergs/s. Iron line fluorescence from an opaque cool (not exceeding 1 million K) shell of material at the Alfven surface provides the necessary luminosity in this feature. The double line structure and the line energy width can be due to Doppler shifts if the shell is forced to corotate with the pulsar at a radius of at least 800 million cm. Implications of this model regarding physical conditions near Her X-1 are discussed.

  12. Possible use of pattern recognition for the analysis of Mars rover X ray fluorescence spectra

    NASA Astrophysics Data System (ADS)

    Trombka, Jacob I.; Seltzer, Stephen M.; Johnson, Robert G.; Philpotts, John A.

    1989-10-01

    On the Mars rover sample return mission the rover vehicle will collect and select samples from different locations on the Martial surface to be brought back to Earth for laboratory studies. It is anticipated that an in situ energy-dispersive X ray fluorescence (XRF) spectrometer will be on board the rover. On such a mission, sample selection is of higher priority than in situ quantitative chemical analysis. With this in mind we propose pattern recognition as a simple, direct, and speedy alternative to detailed chemical analysis of the XRF spectra. The validity and efficacy of the pattern recognition technique are demonstrated by the analyses of laboratory XRF spectra obtained from a series of geological samples, in the form both of standardized pressed pellets and as unprepared rocks. It is found that pattern recognition techniques applied to the raw XRF spectra can provide for the same discrimination among samples as knowledge of their actual chemical composition.

  13. Application of x-ray fluorescence analysis to investigation of the composition of gunshot residues

    NASA Astrophysics Data System (ADS)

    Kazimirov, V. I.; Zorin, A. D.; Zanozina, V. F.

    2006-05-01

    We have used x-ray fluorescence analysis to study the elemental composition of gunshot residues from smooth-bore and rifled-bore guns. We have established that it is possible to differentiate between types of projectiles (jacketed/lead), types of primers (corrosive/noncorrosive), and types of propellant powders (black/smokeless) by analysis of the elemental composition of the gunshot residues. We have shown that the mercury content in gunshot residues on the surface of the object carrying the residues steadily decreases as storage time increases. Despite this fact, mercury can be preserved as a component of gunshot residues on the object (cotton cloth) under room conditions for more than 45 days.

  14. Elemental analysis of white electrical tapes by wavelength dispersive X-ray fluorescence spectrometry.

    PubMed

    Sun, Zhenwen; Quan, Yangke; Sun, Yuyou

    2013-10-10

    The aim of this study was to analyze and discriminate electrical tapes using the wavelength dispersive X-ray fluorescence (XRF) spectrometry and statistical techniques. The backings of 46 white electrical tapes were analyzed. A discrimination of 90.4% was performed only by quantitative analysis of major elements (relative ratio of Cl to Ca). Ten distinct groups with a discrimination of 78.9% were yielded only by qualitative analysis of trace elements. Ninety-nine electrical tape pairs which could not be discriminated by major elements were further compared with the characteristics of trace elements. The overall discriminating power of 96.1% was obtained by the combination of quantitative and qualitative analysis. The ability of XRF technique to discriminate different electrical tapes was similar to several well-known methods combined.

  15. X-Ray Fluorescence to Determine Zn in Bolivian Children using Hair Samples

    NASA Astrophysics Data System (ADS)

    Tellería Narvaez, C. A.; Fernández Alcázar, S.; Barrientos Zamora, F. G.; Chungara Castro, J.; Luna Lauracia, I.; Mamani Tola, H.; Mita Peralta, E.; Muñoz Gosálvez, A. O.; Romero Bolaños, L. E.; Ramírez Ávila, G. M.

    2014-06-01

    As a first step in the evaluation of nutritional levels in Bolivian children (8-13 years-old), we carried out X-Ray Fluorescence measurements in hair samples of children belonging to different social classes and living either in rural areas or in cities. The aim of this study is to contribute to health policies tending to improve the global health of children and consequently avoid malnutrition. Our method intends to have maximum reliability and at the same time be as simple as possible from an experimental point of view. Additionally, we use this method to determine some other elements such as Fe, Cu, Pb, As and Hg, the latter three considered as contaminants that could be present in children living in areas which neighbor mines and industries. This work will be complemented by some biological and medical tests.

  16. [Progress in application of microbeam X-ray fluorescence spectroscopy in forensic science].

    PubMed

    Su, Hui-Fang; Liu, Chao; Hu, Sun-Lin; Wang, Song-Cai; Sun, Li-Min; Huang, Wei; Zhang, Xiao-Ting; Li, Shuang-Lin

    2013-02-01

    Microbeam X-ray fluorescence (micro-XRF) spectrometry has been raised as an analytical technique of microbeam during the recent years. With its advantages of high sensitivity, small sample requirement, high testing accuracy and non-destruction, the technique is widely utilized in forensic science. This review bases on recent researches at home and abroad, describes its applications including identification of gunshot residue, visualization of fingerprints, discrimination of drug source, production process, and other material evidences of analysis in crime scene. Thanks to the advances in technology, intelligent and portable micro-XRF equipment has appeared to be applied. It is believed that it may be more popular and frequent in administration of forensic science in the near future.

  17. Performance of a Borehole X-ray Fluorescence Spectrometer for Planetary Exploration

    NASA Technical Reports Server (NTRS)

    Kelliher, Warren C.; Carlberg, Ingrid A.; Elam, W. T.; Willard-Schmoe, Ella

    2008-01-01

    We have designed and constructed a borehole X-ray Fluorescence Spectrometer (XRFS) as part of the Mars Subsurface Access program [1]. It can be used to determine the composition of the Mars regolith at various depths by insertion into a pre-drilled borehole. The primary requirements and performance metrics for the instrument are to obtain parts-per-million (ppm) lower limits of detection over a wide range of elements in the periodic table (Magnesium to Lead). Power consumption during data collection was also measured. The prototype instrument is complete and preliminary testing has been performed. Terrestrial soil Standard Reference Materials were used as the test samples. Detection limits were about 10 weight ppm for most elements, with light elements being higher, up to 1.4 weight percent for magnesium. Power consumption (excluding ground support components) was 12 watts.

  18. [Determination of major elements in superphosphate by X-ray fluorescence spectrometry].

    PubMed

    Rui, Yu-Kui; Li, He; Shen, Jian-Bo; Zhang, Fu-Suo

    2008-11-01

    Phosphate fertilizer is one of the most important fertilizers. The authors determined nine kinds of major elements in superphosphate, the most important phosphate fertilizer, by X-ray fluorescence spectrometry. The detection range of SiO2, Al2O3, TFe2O3, MnO, MgO, CaO, Na2O, K2O and P2O5 is 15.0%-90.0%, 0.20%-25.0%, 0.20%-25.0%, 0.01%-0.35%, 0.20%-40.0%, 0.10%-35.0%, 0.10%-7.50%, 0.05%-7.50% and 1.00%-100.00% respectively, and the precision of the method for SiO2, Al2O3, TFe2O3, MnO, MgO, CaO, Na2O, K2O and P2O5 range from 0.20% to 0.005%, so the method of X-ray fluorescence spectrometry is a fast and effectual method for detecting the composition of phosphate fertilizer. The contents of the above elements showed (1) the detected superphosphate content is 18.101% of P2O5, which is accordant to the labeled level (> or = 16%); (2) the detected superphosphate contains much SiO2, TFe2O3, MgO, CaO and K2O, which are necessary for plant growth and the content of which is 16.954%, 1.495%, 1.580%, 21.428% and 1.585% respectively. These data showed that phosphate fertilizer sometimes can supply some trace elements for plants, but we should eliminate the interference effect of these elements when we research the role of phosphorus; (3) superphosphate contains 3.225% of Al2O3, so the authors should attention to the aluminium poison when superphosphate is used chronically.

  19. High resolution X-ray fluorescence imaging for a microbeam radiation therapy treatment planning system

    NASA Astrophysics Data System (ADS)

    Chtcheprov, Pavel; Inscoe, Christina; Burk, Laurel; Ger, Rachel; Yuan, Hong; Lu, Jianping; Chang, Sha; Zhou, Otto

    2014-03-01

    Microbeam radiation therapy (MRT) uses an array of high-dose, narrow (~100 μm) beams separated by a fraction of a millimeter to treat various radio-resistant, deep-seated tumors. MRT has been shown to spare normal tissue up to 1000 Gy of entrance dose while still being highly tumoricidal. Current methods of tumor localization for our MRT treatments require MRI and X-ray imaging with subject motion and image registration that contribute to the measurement error. The purpose of this study is to develop a novel form of imaging to quickly and accurately assist in high resolution target positioning for MRT treatments using X-ray fluorescence (XRF). The key to this method is using the microbeam to both treat and image. High Z contrast media is injected into the phantom or blood pool of the subject prior to imaging. Using a collimated spectrum analyzer, the region of interest is scanned through the MRT beam and the fluorescence signal is recorded for each slice. The signal can be processed to show vascular differences in the tissue and isolate tumor regions. Using the radiation therapy source as the imaging source, repositioning and registration errors are eliminated. A phantom study showed that a spatial resolution of a fraction of microbeam width can be achieved by precision translation of the mouse stage. Preliminary results from an animal study showed accurate iodine profusion, confirmed by CT. The proposed image guidance method, using XRF to locate and ablate tumors, can be used as a fast and accurate MRT treatment planning system.

  20. Identifying microbial habitats in soil using quantum dots and x-ray fluorescence microtomography

    NASA Astrophysics Data System (ADS)

    O'Brien, S. L.; Whiteside, M. D.; Sholto-Douglas, D.; Dohnalkova, A.; Durall, D. M.; Gursoy, D.; Jones, M. D.; Kovarik, L.; Lai, B.; Roehrig, C.; Sullivan, S.; Vogt, S.; Kemner, K. M.

    2015-12-01

    The metabolic activities of soil microbes are the primary drivers of biogeochemical processes controlling the terrestrial carbon cycle, nutrient availability to plants, contaminant remediation, water quality, and other ecosystem services. However, we have a limited understanding of microbial metabolic processes such as nutrient uptake rates, substrate preferences, or how microbes and microbial metabolism are distributed throughout the three-dimensional pore network of the soil. Here we use a novel combination of imaging techniques with quantum dots (QDs, engineered semiconductor nanoparticles that produce size or composition-dependent fluorescence) to locate bacteria in the three-dimensional pore network of a soil aggregate. First, we show using confocal and aberration-corrected transmission electron microscopies that bacteria (Bacillus subtilis, Pseudomonas fluorescens, and Pseudomonas protogens) actively take up and internalize CdSe/ZnS core/shell QDs conjugated to biologically relevant substrates. Next, we show that cells bearing QDs can be identified using fluorescence imaging with hard x-rays at 2ID-D at the Advanced Photon Source (APS). Finally, we demonstrate that the Se constituent to the QDs can be used to label bacteria in three-dimensional tomographic reconstructions of natural soil at 0.5 nm spatial resolution using hard x-rays at 2ID-E at the APS. This is the first time soil bacteria have been imaged in the intact soil matrix at such high resolution. These results offer a new way to experimentally investigate basic bacterial ecology in situ, revealing constraints on microbial function in soil that will help improve connections between pore-scale and ecosystem-scale processes in models.

  1. Bromine and bromide content in soils: Analytical approach from total reflection X-ray fluorescence spectrometry.

    PubMed

    Gallardo, Helena; Queralt, Ignasi; Tapias, Josefina; Candela, Lucila; Margui, Eva

    2016-08-01

    Monitoring total bromine and bromide concentrations in soils is significant in many environmental studies. Thus fast analytical methodologies that entail simple sample preparation and low-cost analyses are desired. In the present work, the possibilities and drawbacks of low-power total reflection X-ray fluorescence spectrometry (TXRF) for the determination of total bromine and bromide contents in soils were evaluated. The direct analysis of a solid suspension using 20 mg of fine ground soil (<63 μm) gave a 3.7 mg kg(-1) limit of detection for bromine which, in most cases, was suitable for monitoring total bromine content in soils (Br content range in soils = 5-40 mg kg(-1)). Information about bromide determination in soils is also possible by analyzing the Br content in water soil extracts. In this case, the TXRF analysis can be directly performed by depositing 10 μL of the internal standardized soil extract sample on a quartz glass reflector in a measuring time of 1500 s. The bromide limit of detection by this approach was 10 μg L(-1). Good agreement was obtained between the TXRF results for the total bromine and bromide determinations in soils and those obtained by other popular analytical techniques, e.g. energy dispersive X-ray fluorescence spectrometry (total bromine) and ionic chromatography (bromide). As a study case, the TXRF method was applied to study bromine accumulation in two agricultural soils fumigated with a methyl bromide pesticide and irrigated with regenerated waste water.

  2. Characterization of X-ray polycapillary optics by LiF crystal radiation detectors through confocal fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Bonfigli, Francesca; Hampai, Dariush; Dabagov, Sultan B.; Montereali, Rosa Maria

    2016-08-01

    Solid-state radiation imaging detectors based on photoluminescent colour centres in lithium fluoride (LiF) crystals have been successfully tested for both advanced 2D and 3D characterizations of X-ray polycapillary optics by a table-top laboratory system. Polycapillary optics can control X-ray beams propagation and allows obtaining quasi-parallel beam (half-lens) or focused beams (full-lens). The combination of a fine-focused micro X-ray tube and a polycapillary lens can provide the high intensity radiation fluxes that are necessary for high resolution X-ray imaging. In this paper we present novel results about advanced characterization of these complex optics by 2D as well as 3D confocal laser fluorescence microscopy of X-ray irradiated LiF crystal detectors. Two dimensional high spatial resolution images on a wide field of view of transmitted X-rays through a semi-lens and 3D direct inspection of the coloured volumes produced in LiF crystals by both focused and parallel X-ray beam transmitted by a full and a semi-lens, respectively, as well as their 3D reconstructions were obtained. The results show that the photoluminescent colour centres volume in LiF crystals combined with an optical sectioning reading system provide information about tomography of transmitted X-ray beams by policapillary optics in a single exposure process. For the first time, the use of LiF crystal plates as versatile radiation imaging luminescent detectors have been used to characterize the operation of polycapillary optics as X-ray lens, in focusing and parallel mode.

  3. Rayleigh scattering of two x-ray photons by an atom

    NASA Astrophysics Data System (ADS)

    Hopersky, Alexey N.; Nadolinsky, Alexey M.; Novikov, Sergey A.

    2016-05-01

    The process of elastic (Rayleigh) scattering of two x-ray free-electron laser (XFEL) photons by a free He atom is theoretically investigated. We obtain the absolute values and the forms of the triple differential scattering cross section. The main theoretical result is the highest probability of creation of scattered photons with energy ℏ ω±≅ℏ ω ±I1 s (ℏ ω is the energy of the incident XFEL photon, I1 s is the energy of the ionization threshold of the 1 s2 atomic shell). The probability of creation cooled (<ω- ) and hot (>ω+ ) photons is smaller by many orders of magnitude, and is identically zero when the formal (nonphysical) energy of one of the scattered photons is 2 ℏ ω .

  4. Distribution and speciation of bromine in mammalian tissue and fluids by X-ray fluorescence imaging and X-ray absorption spectroscopy.

    PubMed

    Ceko, Melanie J; Hummitzsch, Katja; Hatzirodos, Nicholas; Bonner, Wendy; James, Simon A; Kirby, Jason K; Rodgers, Raymond J; Harris, Hugh H

    2015-05-01

    Bromine is one of the most abundant and ubiquitous trace elements in the biosphere and until recently had not been shown to perform any essential biological function in animals. A recent study demonstrated that bromine is required as a cofactor for peroxidasin-catalysed formation of sulfilimine crosslinks in Drosophila. In addition, bromine dietary deficiency is lethal in Drosophila, whereas bromine replenishment restores viability. The aim of this study was to examine the distribution and speciation of bromine in mammalian tissues and fluids to provide further insights into the role and function of this element in biological systems. In this study we used X-ray fluorescence (XRF) imaging and inductively coupled plasma-mass spectrometry (ICP-MS) to examine the distribution of bromine in bovine ovarian tissue samples, follicular fluid and aortic serum, as well as human whole blood and serum and X-ray absorption spectroscopy (XAS) to identify the chemical species of bromine in a range of mammalian tissue (bovine, ovine, porcine and murine), whole blood and serum samples (bovine, ovine, porcine, murine and human), and marine samples (salmon (Salmo salar), kingfish (Seriola lalandi) and Scleractinian coral). Bromine was found to be widely distributed across all tissues and fluids examined. In the bovine ovary in particular it was more concentrated in the sub-endothelial regions of arterioles. Statistical comparison of the near-edge region of the X-ray absorption spectra with a library of bromine standards led to the conclusion that the major form of bromine in all samples analysed was bromide.

  5. 2D/3D cryo x-ray fluorescence imaging at the bionanoprobe at the advanced photon source

    SciTech Connect

    Chen, S. Vine, D. J.; Lai, B.; Paunesku, T.; Yuan, Y.; Woloschak, G. E.; Deng, J.; Jin, Q.; Hong, Y. P.; Flachenecker, C.; Hornberger, B.; Brister, K.; Jacobsen, C.; Vogt, S.

    2016-01-28

    Trace elements, particularly metals, play very important roles in biological systems. Synchrotron-based hard X-ray fluorescence microscopy offers the most suitable capabilities to quantitatively study trace metals in thick biological samples, such as whole cells and tissues. In this manuscript, we have demonstrated X-ray fluorescence imaging of frozen-hydrated whole cells using the recent developed Bionanoprobe (BNP). The BNP provides spatial resolution down to 30 nm and cryogenic capabilities. Frozen-hydrated biological cells have been directly examined on a sub-cellular level at liquid nitrogen temperatures with minimal sample preparation.

  6. Production of the ideal sample shape for Total Reflection X-ray Fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Horntrich, C.; Kregsamer, P.; Prost, J.; Stadlbauer, F.; Wobrauschek, P.; Streli, C.

    2012-11-01

    Total Reflection X-ray Fluorescence analysis (TXRF) is a well-established analytical method in the semiconductor industry for the analysis of silicon wafer surfaces. For the calibration of the spectrometer typically an external standard is used which is sensitive to quantification errors. In general TXRF is known to allow for linear calibration. For small sample amounts (pg to ng region) the thin film approximation is valid neglecting absorption effects of the exciting and the detected radiation. For higher total amounts of sample the relation between fluorescence intensity and sample amount diverges from linearity (saturation effect). These deviations lead to difficulties in quantification with external standard. Content of the presented work is the production of the ideal TXRF sample shape, which was theoretically determined to be ring shaped. A possibility for the production of samples with ring shape is the use of a nanodispensing system combined with a positioning device. Therewith it is possible to produce ring shaped samples in a controlled way with the ring consisting of individual nanodroplets, so that the wanted diameter of the ring can be chosen. A comparison of the fluorescence intensities emitted by contracted and ring shaped samples shows that the ring shape is not only theoretically the best TXRF shape but also experimentally. It could be proven that for contracted samples the saturation effect occurs at a lower sample mass than for samples with ring shape.

  7. First use of portable system coupling X-ray diffraction and X-ray fluorescence for in-situ analysis of prehistoric rock art.

    PubMed

    Beck, L; Rousselière, H; Castaing, J; Duran, A; Lebon, M; Moignard, B; Plassard, F

    2014-11-01

    Study of prehistoric art is playing a major role in the knowledge of human evolution. Many scientific methods are involved in this investigation including chemical analysis of pigments present on artefacts or applied to cave walls. In the past decades, the characterization of coloured materials was carried on by taking small samples. This procedure had two main disadvantages: slight but existing damage of the paintings and limitation of the number of samples. Thanks to the advanced development of portable systems, in-situ analysis of pigment in cave can be now undertaken without fear for this fragile Cultural Heritage. For the first time, a portable system combining XRD and XRF was used in an underground and archaeological environment for prehistoric rock art studies. In-situ non-destructive analysis of black prehistoric drawings and determination of their composition and crystalline structure were successfully carried out. Original results on pigments used 13,000 years ago in the cave of Rouffignac (France) were obtained showing the use of two main manganese oxides: pyrolusite and romanechite. The capabilities of the portable XRD-XRF system have been demonstrated for the characterization of pigments as well as for the analysis of rock in a cave environment. This first in-situ experiment combining X-ray diffraction and X-ray fluorescence open up new horizons and can fundamentally change our approach of rock art studies.

  8. [Analysis and characterization of Belamcanda chinensis with space mutagenesis breeding by X-ray fluorescence analysis and X-ray diffraction].

    PubMed

    Guan, Ying; Ding, Xi-Feng; Wang, Wen-Jing; Guo, Xi-Hua; Zhu, Yan-Ying

    2008-02-01

    The contents of various elements in the fourth generation Belamcanda chinensis (L.) DC. with space mutagenesis breeding were analyzed and characterized. X-ray fluorescence spectrum analysis (XRF) and powder X-ray diffraction (PXRD) were applied jointly. It was found that the content of K element in the space flight mutagenesis increases 1.03 and 0.31 times, Mg enhances 1.44 and 0.06 times, but Al reduces 38.5% and 85.5% respectively compared to the contents in the ground group and the comparison group, while those of Ca, Mn and Fe enhance 0.95, 0.30 and 0.29 times respectively contrasted to the ground group. Besides, there was discovered the crystal of whewellite in the Belamcanda chinensis (L.) DC. and the content in the ground group is less than that of the outer space and the outer space group, which in turn is less than that of the comparison group. It is concluded that the contents of mineral elements indispensable to body in the space group are closer or superior to the comparison, group as compared to the ground group. In the present paper, a quick and simple appraising method is offered, which may be of great significance to the popularization of the planting outer space Chinese traditional medicine to filtrate more excellent breed and set up norm of quality appraisal.

  9. Iron speciation in human cancer cells by K-edge total reflection X-ray fluorescence-X-ray absorption near edge structure analysis

    NASA Astrophysics Data System (ADS)

    Polgári, Zs.; Meirer, F.; Sasamori, S.; Ingerle, D.; Pepponi, G.; Streli, C.; Rickers, K.; Réti, A.; Budai, B.; Szoboszlai, N.; Záray, G.

    2011-03-01

    X-ray absorption near edge structure (XANES) analysis in combination with synchrotron radiation induced total reflection X-ray fluorescence (SR-TXRF) acquisition was used to determine the oxidation state of Fe in human cancer cells and simultaneously their elemental composition by applying a simple sample preparation procedure consisting of pipetting the cell suspension onto the quartz reflectors. XANES spectra of several inorganic and organic iron compounds were recorded and compared to that of different cell lines. The XANES spectra of cells, independently from the phase of cell growth and cell type were very similar to that of ferritin, the main Fe store within the cell. The spectra obtained after CoCl 2 or NiCl 2 treatment, which could mimic a hypoxic state of cells, did not differ noticeably from that of the ferritin standard. After 5-fluorouracil administration, which could also induce an oxidative-stress in cells, the absorption edge position was shifted toward higher energies representing a higher oxidation state of Fe. Intense treatment with antimycin A, which inhibits electron transfer in the respiratory chain, resulted in minor changes in the spectrum, resembling rather the N-donor Fe-α,α'-dipyridyl complex at the oxidation energy of Fe(III), than ferritin. The incorporation of Co and Ni in the cells was followed by SR-TXRF measurements.

  10. Mineralogical analysis of clays in hardsetting soil horizons, by X-ray fluorescence and X-ray diffraction using Rietveld method

    NASA Astrophysics Data System (ADS)

    Prandel, L. V.; Saab, S. C.; Brinatti, A. M.; Giarola, N. F. B.; Leite, W. C.; Cassaro, F. A. M.

    2014-02-01

    Diffraction and spectroscopic techniques have been shown to be suitable for obtaining physical and mineralogical properties in polycrystalline soil samples, and also in their precursor compounds. For instance, the X-ray fluorescence (XRF) spectroscopy allows obtaining the elemental composition of an investigated sample, while the X-ray diffraction (XRD) technique permits obtaining qualitative and quantitative composition of the soil minerals through the Rietveld method (RM). In this study Yellow Latosol (Oxisol), Yellow Argisol (Ultisol) and Gray Argisol (Ultisol) soil samples, classified as "hardsetting soils", extracted from areas located at Northeast and Southeast of Brazilian coast were investigated. The soils and their fractions were analyzed in an EDX-700 and an XRD-6000 (Cu Kα radiation). XRF results indicate high percentages of Si and Al, and small percentage of Fe and Ti in the investigated samples. The DRX data and RM indicate that there was a predominance of kaolinite and halloysite minerals (kaolin group minerals) in the clay fractions, which are presumably responsible for the formation of kaolinitic plasma in these soils. Also, the obtained results showed that the XRF, XRD techniques and RM were very helpful for investigating the mineralogical composition of a hardsetting soil.

  11. Impurity precipitation in atomized particles evidenced by nano x-ray diffraction computed tomography

    SciTech Connect

    Bonnin, Anne; Wright, Jonathan P.; Tucoulou, Rémi; Palancher, Hervé

    2014-08-25

    Performances and physical properties of high technology materials are influenced or even determined by their initial microstructure and by the behavior of impurity phases. Characterizing these impurities and their relations with the surrounding matrix is therefore of primary importance but it unfortunately often requires a destructive approach, with the risk of misinterpreting the observations. The improvement we have done in high resolution X-ray diffraction computed tomography combined with the use of an X-ray nanoprobe allows non-destructive crystallographic description of materials with microscopic heterogeneous microstructure (with a grain size between 10 nm and 10 μm). In this study, the grain localization in a 2D slice of a 20 μm solidified atomized γU-Mo particle is shown and a minority U(C,O) phase (1 wt. %) with sub-micrometer sized grains was characterized inside. Evidence is presented showing that the onset of U(C,O) grain crystallization can be described by a precipitation mechanism since one single U-Mo grain has direct orientation relationship with more than one surrounding U(C,O) grains.

  12. Ordered many-electron motions in atoms and x-ray lasers. [Subpicosecond ultraviolet laser radiation

    SciTech Connect

    Rhodes, C.K.

    1986-01-01

    Subpicosecond ultraviolet laser technology is enabling the exploration of nonlinear atomic interactions with electric field strengths considerably in excess of an atomic unit. As this regime is approached, experiments studying multiple ionization, photoelectron energy spectra, and harmonically produced radiation all exhibit strong nonlinear coupling. Peak total energy transfer rates on the order of approx.2 x 10/sup -4/ W/atom have been observed at an intensity of approx.10/sup 16/ W/cm/sup 2/, and it is expected that energy transfer rates approaching approx.0.1 to 1 W/atom will occur under more extreme conditions for which the ultraviolet electric field E is significantly greater than e/a/sub 0//sup 2/. In this high intensity regime, a wide range of new nonlinear phenomena will be open to study. These will include the possibility of ordered driven motions in atoms, molecules, and plasmas, mechanisms involving collisions, and relativistic processes such as electron-positron pair production. An understanding of these physical interactions may provide a basis for the generation of stimulated emission in the x-ray range. 100 refs., 8 figs.

  13. Depth Profile of Mn in GaAs/Mn/GaAs Heterostuctures and Thermal Annealing Effects Studied by Angular Dependence of X-ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Kim, S.; Soo, Y. L.; Kioseoglou, G.; Chen, X.; Luo, H.; Kao, Y. H.; Sasaki, Y.; Liu, X.; Furdyna, J. K.

    2003-03-01

    Angular dependence of x-ray fluorescence (ADXRF) technique has been utilized to study Mn depth profile in GaAs (60 ÅMn (5 Åstructures MBE-grown on GaAs and annealed at temperatures 350, 450, and 550^oC. The nominal structure for as-grown sample was confirmed from detailed fluorescence analysis. We have found that a large amount of Mn migrate into the top GaAs layer in the sample annealed at 550^oC while the other samples showed only a slight change in the Mn profile as compared to the as-grown sample. These results provide unique information on the depth distribution of Mn atoms in Mn/GaAs magnetic digital alloys as a function of temperature in addition to those obtained previously^1 by means of grazing incidence x-ray scattering (GIXS) and x-ray diffraction. We have thus demonstrated that ADXRF technique is a useful nondestructive tool for probing the depth profile of samples with an ultra thin overlay or containing a small amount of impurity atoms. 1. G. Kioseoglou, S. Kim, Y. L. Soo, X. Chen, H. Luo, Y. H. Kao, Y. Sasaki, X. Liu, and J. K. Furdyna, Appl. Phys. Lett. 80, 1150 (2002).

  14. X-Ray Fluorescence Solvent Detection at the Substrate-Adhesive Interface

    NASA Technical Reports Server (NTRS)

    Wurth, Laura; Evans, Kurt; Weber, Bart; Headrick, Sarah

    2005-01-01

    tag element can then be mapped by its characteristic x-ray emission using either x-ray fluorescence, or electron-beam energy-and wavelength-dispersive x-ray spectrometry. The direct mapping techniques avoid issues of different diffusion or migration rates of solvents and elemental tags, while the indirect techniques avoid spectral resolution issues in cases where solvents and substrates have adjacent or overlapping peaks. In this study, cross-section component indirect mapping is being evaluated as a method for measuring migration of d-limonene based solvents in glass-cloth phenolic composite (GCP) prior to and during subsequent bonding and epoxy adhesive cure.

  15. Immediate screening of lead exposure in the workplace using portable X-ray fluorescence

    PubMed Central

    Gorce, Jean-Philippe; Roff, Martin

    2016-01-01

    ABSTRACT The use of a portable X-ray fluorescence spectrometer (PXRF) equipped with a miniaturised X-ray tube producing a small 8 mm diameter X-ray beam required the validation of two new sampling protocols for the immediate screening of occupational lead exposure. First, lead in dust and fumes, collected by Institute of Occupational Medicine (IOM) inhalable samplers on 25 mm diameter membrane filters, is quantified using PXRF. To account for irregular dust deposition, the filters are rotated manually by quarter turns. Multiple PXRF readings are collected from the central region and from two locations in the outer region. The inner region is distinguishable from the outer region, but the two outer region locations are indistinguishable. High correlations (R2 > 0.99) are found between the PXRF results and historical results obtained using a reference method based on a laboratory wavelength-dispersive sequential XRF instrument (WDXRF) for lead loadings between 1–161 μg. The PXRF results from the outer regions of the filters show a bias of −13% with respect to the WDXRF. Once this bias is allowed for, 95% of all PXRF results lie within −28% and +38% of the WDXRF results. Neither instrument accounts for potential dust accumulation on the walls of the IOM sampler. Therefore, methods based on their use can only be considered semi-quantitative. Second, a protocol combining direct PXRF measurements on workplace surfaces with surface wipes is designed for immediate on-site quantification of removable surface lead residues. The quantification of such residues by this method is compared with subsequent off-site wet chemistry analysis of the surface wipes. The two methods show a good correlation (R2 ∼ 0.88). The ratio of the amount of removable residues determined by PXRF and wipe sampling is close to one with range 0.26–3.94. It is demonstrated that PXRF can be used as an effective tool for the immediate screening of occupational lead exposure. Although this

  16. Immediate screening of lead exposure in the workplace using portable X-ray fluorescence.

    PubMed

    Gorce, Jean-Philippe; Roff, Martin

    2016-01-01

    The use of a portable X-ray fluorescence spectrometer (PXRF) equipped with a miniaturised X-ray tube producing a small 8 mm diameter X-ray beam required the validation of two new sampling protocols for the immediate screening of occupational lead exposure. First, lead in dust and fumes, collected by Institute of Occupational Medicine (IOM) inhalable samplers on 25 mm diameter membrane filters, is quantified using PXRF. To account for irregular dust deposition, the filters are rotated manually by quarter turns. Multiple PXRF readings are collected from the central region and from two locations in the outer region. The inner region is distinguishable from the outer region, but the two outer region locations are indistinguishable. High correlations (R(2) > 0.99) are found between the PXRF results and historical results obtained using a reference method based on a laboratory wavelength-dispersive sequential XRF instrument (WDXRF) for lead loadings between 1-161 μg. The PXRF results from the outer regions of the filters show a bias of -13% with respect to the WDXRF. Once this bias is allowed for, 95% of all PXRF results lie within -28% and +38% of the WDXRF results. Neither instrument accounts for potential dust accumulation on the walls of the IOM sampler. Therefore, methods based on their use can only be considered semi-quantitative. Second, a protocol combining direct PXRF measurements on workplace surfaces with surface wipes is designed for immediate on-site quantification of removable surface lead residues. The quantification of such residues by this method is compared with subsequent off-site wet chemistry analysis of the surface wipes. The two methods show a good correlation (R(2) ∼ 0.88). The ratio of the amount of removable residues determined by PXRF and wipe sampling is close to one with range 0.26-3.94. It is demonstrated that PXRF can be used as an effective tool for the immediate screening of occupational lead exposure. Although this article focused on

  17. X-ray nanoprobes and diffraction-limited storage rings: opportunities and challenges of fluorescence tomography of biological specimens

    PubMed Central

    de Jonge, Martin D.; Ryan, Christopher G.; Jacobsen, Chris J.

    2014-01-01

    X-ray nanoprobes require coherent illumination to achieve optic-limited resolution, and so will benefit directly from diffraction-limited storage rings. Here, the example of high-resolution X-ray fluorescence tomography is focused on as one of the most voracious demanders of coherent photons, since the detected signal is only a small fraction of the incident flux. Alternative schemes are considered for beam delivery, sample scanning and detectors. One must consider as well the steps before and after the X-ray experiment: sample preparation and examination conditions, and analysis complexity due to minimum dose requirements and self-absorption. By understanding the requirements and opportunities for nanoscale fluorescence tomography, one gains insight into the R&D challenges in optics and instrumentation needed to fully exploit the source advances that diffraction-limited storage rings offer. PMID:25177992

  18. Novel handheld x-ray fluorescence spectrometer for routine testing for the presence of lead

    NASA Astrophysics Data System (ADS)

    Rensing, Noa M.; Tiernan, Timothy C.; Squillante, Michael R.

    2011-06-01

    RMD is developing a safe, inexpensive, and easy to operate lead detector for retailers and consumers that can reliably detect dangerous levels of lead in toys and other household products. Lead and its compounds have been rated as top chemicals that pose a great threat to human health. However, widespread testing for environmental lead is rarely undertaken until lead poisoning has already been diagnosed. The problem is not due to the accuracy or sensitivity of existing lead detection technology, but rather to the high expense, safety and licensing barriers of available test equipment. An inexpensive and easy to use lead detector would enable the identification of highly contaminated objects and areas and allow for timely and cost effective remediation. The military has similar needs for testing for lead and other heavy elements such as mercury, primarily in the decontamination of former military properties prior to their return to civilian use. RMD's research and development efforts are abased on advanced solid-state detectors combined with recently patented lead detection techniques to develop a consumer oriented lead detector that will be widely available and easy and inexpensive to use. These efforts will result in an instrument that offers: (1) high sensitivity, to identify objects containing dangerous amounts of lead, (2) low cost to encourage widespread testing by consumers and other end users and (3) convenient operation requiring no training or licensing. In contrast, current handheld x-ray fluorescence spectrometers either use a radioactive source requiring licensing and operating training, or use an electronic x-ray source that limits their sensitivity to surface lead.

  19. Portable x-ray fluorescence for the analysis of chromium in nail and nail clippings.

    PubMed

    Fleming, David E B; Ware, Chris S

    2017-03-01

    Assessment of chromium content in human nail or nail clippings could serve as an effective biomarker of chromium status. The feasibility of a new portable x-ray fluorescence (XRF) approach to chromium measurement was investigated through analysis of nail and nail clipping phantoms. Five measurements of 180s (real time) duration were first performed on six whole nail phantoms having chromium concentrations of 0, 2, 5, 10, 15, and 20µg/g. Using nail clippers, these phantoms were then converted to nail clippings, and assembled into different mass groups of 20, 40, 60, 80, and 100mg for additional measurements. The amplitude of the chromium Kα characteristic x-ray energy peak was examined as a function of phantom concentration for all measurement conditions to create a series of calibration lines. The minimum detection limit (MDL) for chromium was also calculated for each case. The chromium MDL determined from the whole nail intact phantoms was 0.88±0.03µg/g. For the clipping phantoms, the MDL ranged from 1.2 to 3.3µg/g, depending on the mass group analyzed. For the 40mg clipping group, the MDL was 1.2±0.1µg/g, and higher mass collections did not improve upon this result. This MDL is comparable to chromium concentration levels seen in various studies involving human nail clippings. Further improvements to the portable XRF technique would be required to detect chromium levels expected from the lower end of a typical population.

  20. Hard X-ray Fluorescence Measurements of Heteroepitaxial Solid Oxide Fuel Cell Cathode Materials

    SciTech Connect

    Davis, Jacob N.; Miara, Lincoln J.; Saraf, Laxmikant V.; Kaspar, Tiffany C.; Gopalan, Srikanth; Pal, Uday B.; Woicik, Joseph C.; Basu, Soumendra N.; Ludwig, Karl F.

    2012-12-01

    Commonly, SOFCs are operated at high temperatures (above 800°C). At these temperatures expensive housing is needed to contain an operating stack as well as coatings to contain the oxidation of the metallic interconnects. Lowering the temperature of an operating device would allow for more conventional materials to be used, thus lowering overall cost. Understanding the surface chemical states of cations in the surface of the SOFC cathode is vital to designing a system that will perform well at lower temperatures. The samples studied were grown by pulsed laser deposition (PLD) at the Environmental Molecular Sciences Laboratory (EMSL) at Pacific Northwest National Laboratory (PNNL). 20% strontium doped lanthanum manganite (LSM-20) was grown on YSZ and NGO (neodymium gallate). The films on YSZ have a fiber texture. LSM-20 on NGO is heteroepitaxial. Lanthanum strontium cobalt ferrite (LSCF-6428) films were grown on LAO and YSZ with a GDC barrier layer. Total X-ray Reflection Fluorescence (TXRF) was used to depth profile the samples. In a typical experiment, the angle of the incident beam is varied though the critical angle. Below the critical angle, the x-ray decays as an evanescent wave and will only penetrate the top few nanometers. TXRF experiments done on LSM films have suggested strontium segregates to the surface and form strontium enriched nanoparticles (1). It should be pointed out that past studies have focused on 30% strontium A-site doping, but this project uses 20% strontium doped lanthanum manganite. XANES and EXAFS data were taken as a function of incoming angle to probe composition as a function of depth. XANES spectra can be difficult to analyze fully. For other materials density functional theory calculations compared to near edge measurements have been a good way to understand the 3d valence electrons (2).

  1. Rapid and reliable diagnosis of Wilson disease using X-ray fluorescence.

    PubMed

    Kaščáková, Slávka; Kewish, Cameron M; Rouzière, Stéphan; Schmitt, Françoise; Sobesky, Rodolphe; Poupon, Joël; Sandt, Christophe; Francou, Bruno; Somogyi, Andrea; Samuel, Didier; Jacquemin, Emmanuel; Dubart-Kupperschmitt, Anne; Nguyen, Tuan Huy; Bazin, Dominique; Duclos-Vallée, Jean-Charles; Guettier, Catherine; Le Naour, François

    2016-07-01

    Wilson's disease (WD) is a rare autosomal recessive disease due to mutations of the gene encoding the copper-transporter ATP7B. The diagnosis is hampered by the variability of symptoms induced by copper accumulation, the inconstancy of the pathognomonic signs and the absence of a reliable diagnostic test. We investigated the diagnostic potential of X-ray fluorescence (XRF) that allows quantitative analysis of multiple elements. Studies were performed on animal models using Wistar rats (n = 10) and Long Evans Cinnamon (LEC) rats (n = 11), and on human samples including normal livers (n = 10), alcohol cirrhosis (n = 8), haemochromatosis (n = 10), cholestasis (n = 6) and WD (n = 22). XRF experiments were first performed using synchrotron radiation to address the elemental composition at the cellular level. High-resolution mapping of tissue sections allowed measurement of the intensity and the distribution of copper, iron and zinc while preserving the morphology. Investigations were further conducted using a laboratory X-ray source for irradiating whole pieces of tissue. The sensitivity of XRF was highlighted by the discrimination of LEC rats from wild type even under a regimen using copper deficient food. XRF on whole formalin-fixed paraffin embedded needle biopsies allowed profiling of the elements in a few minutes. The intensity of copper related to iron and zinc significantly discriminated WD from other genetic or chronic liver diseases with 97.6% specificity and 100% sensitivity. This study established a definite diagnosis of Wilson's disease based on XRF. This rapid and versatile method can be easily implemented in a clinical setting.

  2. High energy x-ray diffraction/x-ray fluorescence spectroscopy for high-throughput analysis of composition spread thin films.

    PubMed

    Gregoire, John M; Dale, Darren; Kazimirov, Alexander; DiSalvo, Francis J; van Dover, R Bruce

    2009-12-01

    High-throughput crystallography is an important tool in materials research, particularly for the rapid assessment of structure-property relationships. We present a technique for simultaneous acquisition of diffraction images and fluorescence spectra on a continuous composition spread thin film using a 60 keV x-ray source. Subsequent noninteractive data processing provides maps of the diffraction profiles, thin film fiber texture, and composition. Even for highly textured films, our diffraction technique provides detection of diffraction from each family of Bragg reflections, which affords direct comparison of the measured profiles with powder patterns of known phases. These techniques are important for high throughput combinatorial studies as they provide structure and composition maps which may be correlated with performance trends within an inorganic library.

  3. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates

    PubMed Central

    Huang, H. Y.; Jia, C. J.; Chen, Z. Y.; Wohlfeld, K.; Moritz, B.; Devereaux, T. P.; Wu, W. B.; Okamoto, J.; Lee, W. S.; Hashimoto, M.; He, Y.; Shen, Z. X.; Yoshida, Y.; Eisaki, H.; Mou, C. Y.; Chen, C. T.; Huang, D. J.

    2016-01-01

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O8+δ. Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast, the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors. PMID:26794437

  4. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates

    SciTech Connect

    Huang, H. Y.; Jia, C. J.; Chen, Z. Y.; Wohlfeld, K.; Moritz, B.; Devereaux, T. P.; Wu, W. B.; Okamoto, J.; Lee, W. S.; Hashimoto, M.; He, Y.; Shen, Z. X.; Yoshida, Y.; Eisaki, H.; Mou, C. Y.; Chen, C. T.; Huang, D. J.

    2016-01-22

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O8+δ. Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast, the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors.

  5. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates

    DOE PAGES

    Huang, H. Y.; Jia, C. J.; Chen, Z. Y.; ...

    2016-01-22

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O8+δ. Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast,more » the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors.« less

  6. Lead tolerance and cellular distribution in Elsholtzia splendens using synchrotron radiation micro-X-ray fluorescence.

    PubMed

    Zhang, Jie; Tian, Shengke; Lu, Lingli; Shohag, M J I; Liao, Haibing; Yang, Xiaoe

    2011-12-15

    Hydroponic experiments were conducted to investigate the tolerance and spatial distribution of lead (Pb) in Elsholtzia splendens-a copper (Cu) accumulator plant using synchrotron-based micro-X-ray fluorescence. According to chlorophyll concentration and chlorophyll fluorescence parameters, E. splendens displayed certain tolerance at 100 μM Pb treatment. Lead concentration in roots, stems and leaves of E. splendens reached 45,183.6, 1657.6, and 380.9 mg kg(-1), respectively. Pb was mostly accumulated in the roots, and there were also high concentrations of Pb been transported into stems and leaves. Micro-XRF analysis of the stem and leaf cross section revealed that Pb was mostly restricted in the vascular bundles and epidermis tissues of both stem and leaf of E. splendens. The correlation between distribution of K, Ca, Zn and Pb were analyzed. There were significant positive correlations (P<0.01) among Pb and Ca, K, Zn distribution both in stem and leaf of E. splendens. However, among the three elements, Ca shared the most similar distribution pattern and the highest correlation coefficients with Pb in both stem and leaf cross section of E. splendens. This suggests that Ca may play an important role in Pb accumulation in stem and leaf of E. splendens.

  7. Study of heavy metals in wild edible mushrooms under different pollution conditions by X-ray fluorescence spectrometry.

    PubMed

    Carvalho, M L; Pimentel, A C; Fernandes, B

    2005-07-01

    In this work we studied and compared the metal uptake in edible mushrooms (Lepiota procera, Boletus badius, Boletus edulis, Tricholoma equestry, Lactarius deliciosus, Cantarelus tubalformis and Cantarelus edulis), relative to sampling sites submitted to different pollution conditions: car traffic, soil pollution due to pesticides and fertilizers used in old vineyards, and incineration of hospital waste. Soil was also collected in some places, and its content was correlated to the corresponding one in some mushrooms species. All samples, without any chemical treatment, were analyzed by an X-ray fluorescence set-up. This technique is based on a monochromatic X-ray beam ionizing the atoms of the sample. Following this ionization, the emitted radiation is characteristic of the element, allowing its identification and quantification. Vineyards are normally submitted to very high amounts of sulfating, containing high copper concentrations. This metal is accumulated on the soil, and can be up-taken by vegetation. Very high levels of Fe and Cu were found in Lepiota procera species in old vineyards. Zinc was found to be always higher than Cu by factors ranging from 1.5 to 8 in clean wood taken as a reference for the whole analyzed species, while in old vineyards the ratio Zn/Cu reach 0.25 for Lepiota procera. This is correlated to the soil content for both elements. In addition, pollution induced by car traffic was checked in some samples, collected in the proximity of highways. Pb was the main contaminant in these areas, and presenting values 10 times higher than the corresponding ones in sites not submitted to pollution, for some species. Mushrooms contamination due to incineration of hospital waste was also studied, but we did not observe any contamination involving heavy metals in the several analyzed species around these areas. This is in agreement with what was expected, taking into account that hospital waste is mostly organic and, in principle, no heavy metals would

  8. Polarizable atomic multipole X-ray refinement: application to peptide crystals

    SciTech Connect

    Schnieders, Michael J.; Fenn, Timothy D.; Pande, Vijay S.; Brunger, Axel T.

    2009-09-01

    A method to accelerate the computation of structure factors from an electron density described by anisotropic and aspherical atomic form factors via fast Fourier transformation is described for the first time. Recent advances in computational chemistry have produced force fields based on a polarizable atomic multipole description of biomolecular electrostatics. In this work, the Atomic Multipole Optimized Energetics for Biomolecular Applications (AMOEBA) force field is applied to restrained refinement of molecular models against X-ray diffraction data from peptide crystals. A new formalism is also developed to compute anisotropic and aspherical structure factors using fast Fourier transformation (FFT) of Cartesian Gaussian multipoles. Relative to direct summation, the FFT approach can give a speedup of more than an order of magnitude for aspherical refinement of ultrahigh-resolution data sets. Use of a sublattice formalism makes the method highly parallelizable. Application of the Cartesian Gaussian multipole scattering model to a series of four peptide crystals using multipole coefficients from the AMOEBA force field demonstrates that AMOEBA systematically underestimates electron density at bond centers. For the trigonal and tetrahedral bonding geometries common in organic chemistry, an atomic multipole expansion through hexadecapole order is required to explain bond electron density. Alternatively, the addition of interatomic scattering (IAS) sites to the AMOEBA-based density captured bonding effects with fewer parameters. For a series of four peptide crystals, the AMOEBA–IAS model lowered R{sub free} by 20–40% relative to the original spherically symmetric scattering model.

  9. Investigations of Silk Fibers Using X-Ray Scattering and Atomic Force Microscopy

    NASA Astrophysics Data System (ADS)

    Miller, Lance D.; Putthanarat, Sirina; Eby, Ronald K.; Adams, W. W.; Liu, G. F.

    1998-03-01

    Silk fibers from the cocoon of Bombyx mori and the dragline of Nephila clavipes have been investigated by small angle x-ray scattering (SAXS) and atomic force microscopy (AFM). The large scale morphology of these silks have minimum scattering dimensions, and correlation length on the order of 150-300 nm. Several types of AFM measurements on peeled and abraided silk samples have revealed dimensions in agreement with SAXS results. Further agreemeent has been found through the incorporation of discrete Fourier transform theory on AFM topographic information as compared to SAXS patterns. This incorporation allows the materials scientist a way of visualizing the relationship between a material and its resulting scattering function. All of these studies yield a more complete view of the silk morphology and give a new method of model building from scattering experiments.

  10. Orthoclase surface structure dissolution measured in situ by x-ray reflectivity and atomic force microscopy.

    SciTech Connect

    Sturchio, N. C.; Fenter, P.; Cheng, L.; Teng, H.

    2000-11-28

    Orthoclase (001) surface topography and interface structure were measured during dissolution by using in situ atomic force microscopy (AFM) and synchrotrons X-ray reflectivity at pH 1.1-12.9 and T = 25-84 C. Terrace roughening at low pH and step motion at high pH were the main phenomena observed, and dissolution rates were measured precisely. Contrasting dissolution mechanisms are inferred for low- and high-pH conditions. These observations clarify differences in alkali feldspar dissolution mechanisms as a function of pH, demonstrate a new in situ method for measuring face-specific dissolution rates on single crystals, and improve the fundamental basis for understanding alkali feldspar weathering processes.

  11. Quantitative imaging of gold nanoparticle distribution in a tumor-bearing mouse using benchtop x-ray fluorescence computed tomography

    NASA Astrophysics Data System (ADS)

    Manohar, Nivedh; Reynoso, Francisco J.; Diagaradjane, Parmeswaran; Krishnan, Sunil; Cho, Sang Hyun

    2016-02-01

    X-ray fluorescence computed tomography (XFCT) is a technique that can identify, quantify, and locate elements within objects by detecting x-ray fluorescence (characteristic x-rays) stimulated by an excitation source, typically derived from a synchrotron. However, the use of a synchrotron limits practicality and accessibility of XFCT for routine biomedical imaging applications. Therefore, we have developed the ability to perform XFCT on a benchtop setting with ordinary polychromatic x-ray sources. Here, we report our postmortem study that demonstrates the use of benchtop XFCT to accurately image the distribution of gold nanoparticles (GNPs) injected into a tumor-bearing mouse. The distribution of GNPs as determined by benchtop XFCT was validated using inductively coupled plasma mass spectrometry. This investigation shows drastically enhanced sensitivity and specificity of GNP detection and quantification with benchtop XFCT, up to two orders of magnitude better than conventional x-ray CT. The results also reaffirm the unique capabilities of benchtop XFCT for simultaneous determination of the spatial distribution and concentration of nonradioactive metallic probes, such as GNPs, within the context of small animal imaging. Overall, this investigation identifies a clear path toward in vivo molecular imaging using benchtop XFCT techniques in conjunction with GNPs and other metallic probes.

  12. Quantitative imaging of gold nanoparticle distribution in a tumor-bearing mouse using benchtop x-ray fluorescence computed tomography

    PubMed Central

    Manohar, Nivedh; Reynoso, Francisco J.; Diagaradjane, Parmeswaran; Krishnan, Sunil; Cho, Sang Hyun

    2016-01-01

    X-ray fluorescence computed tomography (XFCT) is a technique that can identify, quantify, and locate elements within objects by detecting x-ray fluorescence (characteristic x-rays) stimulated by an excitation source, typically derived from a synchrotron. However, the use of a synchrotron limits practicality and accessibility of XFCT for routine biomedical imaging applications. Therefore, we have developed the ability to perform XFCT on a benchtop setting with ordinary polychromatic x-ray sources. Here, we report our postmortem study that demonstrates the use of benchtop XFCT to accurately image the distribution of gold nanoparticles (GNPs) injected into a tumor-bearing mouse. The distribution of GNPs as determined by benchtop XFCT was validated using inductively coupled plasma mass spectrometry. This investigation shows drastically enhanced sensitivity and specificity of GNP detection and quantification with benchtop XFCT, up to two orders of magnitude better than conventional x-ray CT. The results also reaffirm the unique capabilities of benchtop XFCT for simultaneous determination of the spatial distribution and concentration of nonradioactive metallic probes, such as GNPs, within the context of small animal imaging. Overall, this investigation identifies a clear path toward in vivo molecular imaging using benchtop XFCT techniques in conjunction with GNPs and other metallic probes. PMID:26912068

  13. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis.

    PubMed

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Ward, Jesse; Deng, Junjing; Mak, Rachel; Moonier, Nena; Jacobsen, Chris

    2015-01-01

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologically important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results.

  14. Ultraviolet Germicidal Irradiation and Its Effects on Elemental Distributions in Mouse Embryonic Fibroblast Cells in X-Ray Fluorescence Microanalysis

    PubMed Central

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Ward, Jesse; Deng, Junjing; Mak, Rachel; Moonier, Nena; Jacobsen, Chris

    2015-01-01

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologically important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results. PMID:25706293

  15. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis

    DOE PAGES

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; ...

    2015-02-23

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologicallymore » important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results.« less

  16. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis

    SciTech Connect

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Ward, Jesse; Deng, Junjing; Mak, Rachel; Moonier, Nena; Jacobsen, Chris; Brody, James P.

    2015-02-23

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologically important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results.

  17. Relating Intercellular Variability in Nanoparticle Uptake with Biological Consequence: A Quantitative X-ray Fluorescence Study for Radiosensitization of Cells.

    PubMed

    Turnbull, Tyron; Douglass, Michael; Paterson, David; Bezak, Eva; Thierry, Benjamin; Kempson, Ivan

    2015-11-03

    Internalized gold nanoparticles were quantified in large numbers of individual prostate cancer cells using large area synchrotron X-ray fluorescence microscopy. Cells were also irradiated with a 6 MV linear accelerator to assess the biological consequence of radiosensitization with gold nanoparticles. A large degree of heterogeneity in nanoparticle uptake between cells resulted in influenced biological effect.

  18. FIELD MEASUREMENT TECHNOLOGY FOR MERCURY IN SOIL AND SEDIMENT NITON'S XLI/XLT 700 SERIES X-RAY FLUORESCENCE ANALYZER

    EPA Science Inventory

    NITON's XL-700 Series X-ray fluorescence analyzers were demonstrated under the U.S. Environmental Protection Agency Superfund Innovative Technology Evaluation Program in May 2003 at the Oak Ridge National Laboratory (ORNL) in Oak Ridge, Tennessee. The purpose of the Demonstration...

  19. A Review of Energy Dispersive X-Ray Fluorescence (EDXRF) as an Analytical Tool in Numismatic Studies.

    PubMed

    Navas, María José; Asuero, Agustín García; Jiménez, Ana María

    2016-01-01

    Energy dispersive X-ray fluorescence spectrometry (EDXRF) as an analytical technique in studies of ancient coins is summarized and reviewed. Specific EDXRF applications in historical studies, in studies of the corrosion of coins, and in studies of the optimal working conditions of some laser-based treatment for the cleaning of coins are described.

  20. ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT - FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER - METOREX, INC. X-MET 920-P AND 940

    EPA Science Inventory

    In April 1995, the U.S. Environmental Protection Agency (EPA) sponsored a demonstration of field portable X-ray fluorescence (FPXRF) analyzers. The primary objectives of this demonstration were (1) to determine how well FPXRF analyzers perform in comparison to standard reference...

  1. Development of Standard Samples for on-board Calibration of a New Planetary X-Ray Fluorescence Spectrometer

    NASA Astrophysics Data System (ADS)

    Dreißigacker, Anne; Köhler, Eberhard; Fabel, Oliver; van Gasselt, Stephan

    2014-05-01

    At the Planetary Sciences and Remote Sensing research group at Freie Universität Berlin an SCD-based X-Ray Fluorescence Spectrometer is being developed to be employed on planetary orbiters to conduct direct, passive energy-dispersive x-ray fluorescence measurements of planetary surfaces through measuring the emitted X-Ray fluorescence induced by solar x-rays and high energy particles. Because the Sun is a highly variable radiation source, the intensity of solar X-Ray radiation has to be monitored constantly to allow for comparison and signal calibration of X-Ray radiation from lunar surface materials. Measurements are obtained by indirectly monitoring incident solar x-rays emitted from a calibration sample. This has the additional advantage of minimizing the risk of detector overload and damage during extreme solar events such as high-energy solar flares and particle storms as only the sample targets receive the higher radiation load directly (while the monitor is never directly pointing towards the Sun). Quantitative data are being obtained and can be subsequently analysed through synchronous measurement of fluorescence of the Moon's surface by the XRF-S main instrument and the emitted x-ray fluorescence of calibration samples by the XRF-S-ISM (Indirect Solar Monitor). We are currently developing requirements for 3 sample tiles for onboard correction and calibration of XRF-S, each with an area of 3-9 cm2 and a maximum weight of 45 g. This includes development of design concepts, determination of techniques for sample manufacturing, manufacturing and testing of prototypes and statistical analysis of measurement characteristics and quantification of error sources for the advanced prototypes and final samples. Apart from using natural rock samples as calibration sample, we are currently investigating techniques for sample manufacturing including laser sintering of rock-glass on metals, SiO2-stabilized mineral-powders, or artificial volcanic glass. High precision

  2. X-ray fluorescence for quantification of lead and strontium in vivo

    NASA Astrophysics Data System (ADS)

    Specht, Aaron James

    Lead (Pb) is a toxicant well known for its effects on almost every organ system in the body. Pb use in industry has declined since removal of Pb from gasoline, but many developing countries still have significant use of Pb. Exposure to Pb has been linked with diseases causing neurodegeneration and thus have lasting effects long after the initial exposure. Another metal, strontium (Sr), has been linked with bone disease in particular situations and shown to have uses in treating osteoporosis as a supplement. However, there are no studies of the effects of Sr using a meaningful biomarker. The most commonly used biomarkers for Pb and Sr exposures are blood Pb and Sr; however, blood tests are unable to identify long-term exposure levels due to the short half-life of these metals in blood. Bone stores of Pb and Sr have a half-life of years to decades and serve as a biomarker of long-term exposure. X-ray fluorescence has been used to measure bone Pb and Sr. However, current systems have limitations with radioisotope sources, bulky equipment, and long measurement times. A portable XRF device capable of measurement of bone Pb and Sr, overcomes the limitation of the current systems and has been developed in this work. The detection limit of the portable XRF for bone Pb and Sr was found to be 11 ppm and 5 ppm respectively at 5 mm of skin thickness. The portable XRF will have limitations of measurement based on an individual's skin thickness. The device was calibrated using standard phantoms and validated with in-lab samples, which demonstrated good agreement between KXRF and portable XRF measurements with strong correlations between goat bone, cadaver bone, and phantom measurements. In a population study of Pb poisoned children the portable XRF was further validated and a significant correlation between KXRF measured bone Pb and portable XRF measured bone Pb was identified; however, the device had limitations based on anatomical differences unaccounted for in children from

  3. [Application of confocal micro-beam X-ray fluorescence in nondestructive scanning analysis of the distribution of elements in a single hair].

    PubMed

    Liu, He-He; Liu, Zhi-Guo; Sun, Tian-Xi; Peng, Song; Zhao, Wei-Gang; Sun, Wei-Yuan; Li, Yu-De; Lin, Xiao-Yan; Zhao, Guang-Cui; Luo, Ping; Ding, Xun-Liang

    2013-11-01

    The confocal micro X-ray fluorescence (XRF) based on polycapillary X-ray lens and conventional X-ray source was used to carry out the scanning analysis of the distribution of the elements in a single hair. The elemental distribution in the single hair was obtained. In the confocal micro XRF technology, the output focal spot of the polycapillary focusing X-ray lens and the input focal spot of the polycapillary parallel X-ray lens were adjusted confocally. The detector could only detect the X-rays from the overlapping foci. This confocal structure decreased the effects of the background on the X-ray spectra, and was accordingly helpful for improving the accuracy of this XRF technology. A polycapillary focusing X-ray lens with a high gain in power density was used to decrease the requirement of power of the X-ray source used in this confocal technology, and made it possible to perform such confocal micro XRF analysis by using the conventional X-ray source with low cost. Experimental results indicated that the confocal micro X-ray fluorescence based on polycapillary X-ray lens had potential applications in analyzing the elemental distribution of individual hairs.

  4. Watershed-Scale Geochemical Inventory of Soils by Portable X-Ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Beaudette, D. E.; Stupi, L. K.; Swarowsky, A.; O'Geen, A. T.; Chang, J. F.; Gallagher, B.

    2009-12-01

    Spatial databases of geochemical data are an excellent source of point-scale information on naturally occurring toxic elements (arsenic, selenium or radon), contamination from industrial processes (lead, mercury, or cesium), mineralogical variability, and the fate of toxic compounds (i.e. sorption of pesticides to iron oxyhydroxide minerals) in soil. Sample preparation time, safety concerns associated with HF or HNO3 acid dissolution, instrument availability, and cost are all common constraints that limit the scale at which new geochemical surveys can be conducted. We used a Thermo-Fisher Niton portable X-Ray fluorescence (XRF) meter to perform comparatively rapid geochemical surveys in soils of two (35 ha) watersheds. The watersheds have contrasting parent materials, one formed from metavolcanic rock and the other from granite. The X-Ray fluorescence inventory of genetic soil horizons (n=660) was used to identify trends in soil development and landscape processes. Since soil samples are usually sieved and ground for standard laboratory characterization, the additional time required to prepare samples for XRF analysis was minimal, approximately 2 minutes for sample preparation and 6 minutes for machine scan time per sample. Preliminary analysis of the resulting geochemical data show strong spatial trends in watershed- and hillslope-scale variability in weathering indices (FeCBD:FeTotal and K:Ti), inferred mineralogy (Si:Al, Si:Al+Fe), and geologic signatures (multivariate analysis of 20 common elements). Depth trends and spatial patterns were correlated with common terrain-shape indices (slope, upslope contributing area, surface curvatures, local prominence, etc.), degree of soil development, parent material, and hydrological conditions. For example, Si:Al was higher in soils with greater upslope contributing area, and in seasonally saturated soils (Fig 1). Our findings demonstrate that portable XRF technology is a promising new tool for rapid lab-based and in situ

  5. Gemas: issues from the comparison of aqua regia and X-ray fluorescence results

    NASA Astrophysics Data System (ADS)

    Dinelli, Enrico; Birke, Manfred; Reimann, Clemens; Demetriades, Alecos; DeVivo, Benedetto; Flight, Dee; Ladenberger, Anna; Albanese, Stefano; Cicchella, Domenico; Lima, Annamaria

    2014-05-01

    The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution in soil. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database, consisting of 2 x ca. 2100 samples spread evenly over 33 European countries, is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the Geological Survey of the Slovak Republic, AR analyses were carried out at ACME Labs, and XRF analyses at the Federal Institute for Geosciences and Natural Resources, Germany Element recovery by AR is very different, ranging from <1% (e.g. Na, Zr) to > 80% (e.g. Mn, P, Co). Recovery is controlled by mineralogy of the parent material, but geographic and climatic factors and the weathering history of the soils are also important. Nonetheless, even the very low recovery elements show wide ranges of variation and spatial patterns that are affected by other factors than soil parent material. For many elements soil pH have a clear influence on AR extractability: under acidic soil conditions almost all elements tend to be leached and their extractability is generally low. It progressively increases with increasing pH and is highest in the pH range 7-8. Critical is the clay content of the soil

  6. Probing the graphite band structure with resonant soft-x-ray fluorescence

    SciTech Connect

    Carlisle, J.A.; Shirley, E.L.; Hudson, E.A.

    1997-04-01

    Soft x-ray fluorescence (SXF) spectroscopy using synchrotron radiation offers several advantages over surface sensitive spectroscopies for probing the electronic structure of complex multi-elemental materials. Due to the long mean free path of photons in solids ({approximately}1000 {angstrom}), SXF is a bulk-sensitive probe. Also, since core levels are involved in absorption and emission, SXF is both element- and angular-momentum-selective. SXF measures the local partial density of states (DOS) projected onto each constituent element of the material. The chief limitation of SXF has been the low fluorescence yield for photon emission, particularly for light elements. However, third generation light sources, such as the Advanced Light Source (ALS), offer the high brightness that makes high-resolution SXF experiments practical. In the following the authors utilize this high brightness to demonstrate the capability of SXF to probe the band structure of a polycrystalline sample. In SXF, a valence emission spectrum results from transitions from valence band states to the core hole produced by the incident photons. In the non-resonant energy regime, the excitation energy is far above the core binding energy, and the absorption and emission events are uncoupled. The fluorescence spectrum resembles emission spectra acquired using energetic electrons, and is insensitive to the incident photon`s energy. In the resonant excitation energy regime, core electrons are excited by photons to unoccupied states just above the Fermi level (EF). The absorption and emission events are coupled, and this coupling manifests itself in several ways, depending in part on the localization of the empty electronic states in the material. Here the authors report spectral measurements from highly oriented pyrolytic graphite.

  7. Total reflection X-ray fluorescence trace mercury determination by trapping complexation: Application in advanced oxidation technologies

    NASA Astrophysics Data System (ADS)

    Custo, Graciela; Litter, Marta I.; Rodríguez, Diana; Vázquez, Cristina

    2006-11-01

    It is well known that Hg species cause high noxious effects on the health of living organisms even at very low levels (5 μg/L). Quantification of this element is an analytical challenge due to the peculiar physicochemical properties of all Hg species. The regulation of the maximal allowable Hg concentration led to search for sensitive methods for its determination. Total reflection X-ray fluorescence is a proved instrumental analytical tool for the determination of trace elements. In this work, the use of total reflection X-ray fluorescence for Hg quantification is investigated. However, experimental determination by total reflection X-ray fluorescence requires depositing a small volume of sample on the reflector and evaporation of the solvent until dryness to form a thin film. Because of volatilization of several Hg forms, a procedure to capture these volatile species in liquid samples by using complexing agents is proposed. Acetate, oxalic acid, ethylenediaminetetracetic acid and ammonium pyrrolidine-dithiocarbamate were assayed for trapping the analytes into the solution during the preparation of the sample and onto the reflector during total reflection X-ray fluorescence measurements. The proposed method was applied to evaluate Hg concentration during TiO 2-heterogeneous photocatalysis, one of the most known advanced oxidation technologies. Advanced oxidation technologies are processes for the treatment of effluents in waters and air that involve the generation of very active oxidative and reductive species. In heterogeneous photocatalysis, Hg is transformed to several species under ultraviolet illumination in the presence of titanium dioxide. Total reflection X-ray fluorescence was demonstrated to be applicable in following the extent of the heterogeneous photocatalysis reaction by determining non-transformed Hg in the remaining solution.

  8. A study of ancient pottery by means of X-ray fluorescence spectroscopy, multivariate statistics and mineralogical analysis.

    PubMed

    Papachristodoulou, Christina; Oikonomou, Artemios; Ioannides, Kostas; Gravani, Konstantina

    2006-07-28

    Energy-dispersive X-ray fluorescence spectroscopy was used to determine the composition of 64 potsherds from the Hellenistic settlement of Orraon, in northwestern Greece. Data classification by principal components analysis revealed four distinct groups of pottery, pointing to different local production practices rather than different provenance. The interpretation of statistical grouping was corroborated by a complementary X-ray diffraction analysis. Compositional and mineralogical data, combined with archaeological and materials' science criteria, allowed addressing various aspects of pottery making, such as selection of raw clays, tempers and firing conditions.

  9. Analytic 3D Imaging of Mammalian Nucleus at Nanoscale Using Coherent X-Rays and Optical Fluorescence Microscopy

    PubMed Central

    Song, Changyong; Takagi, Masatoshi; Park, Jaehyun; Xu, Rui; Gallagher-Jones, Marcus; Imamoto, Naoko; Ishikawa, Tetsuya

    2014-01-01

    Despite the notable progress that has been made with nano-bio imaging probes, quantitative nanoscale imaging of multistructured specimens such as mammalian cells remains challenging due to their inherent structural complexity. Here, we successfully performed three-dimensional (3D) imaging of mammalian nuclei by combining coherent x-ray diffraction microscopy, explicitly visualizing nuclear substructures at several tens of nanometer resolution, and optical fluorescence microscopy, cross confirming the substructures with immunostaining. This demonstrates the successful application of coherent x-rays to obtain the 3D ultrastructure of mammalian nuclei and establishes a solid route to nanoscale imaging of complex specimens. PMID:25185543

  10. Fast automatic segmentation of anatomical structures in x-ray computed tomography images to improve fluorescence molecular tomography reconstruction

    NASA Astrophysics Data System (ADS)

    Freyer, Marcus; Ale, Angelique; Schulz, Ralf B.; Zientkowska, Marta; Ntziachristos, Vasilis; Englmeier, Karl-Hans

    2010-05-01

    The recent development of hybrid imaging scanners that integrate fluorescence molecular tomography (FMT) and x-ray computed tomography (XCT) allows the utilization of x-ray information as image priors for improving optical tomography reconstruction. To fully capitalize on this capacity, we consider a framework for the automatic and fast detection of different anatomic structures in murine XCT images. To accurately differentiate between different structures such as bone, lung, and heart, a combination of image processing steps including thresholding, seed growing, and signal detection are found to offer optimal segmentation performance. The algorithm and its utilization in an inverse FMT scheme that uses priors is demonstrated on mouse images.

  11. Normal incidence x-ray mirror for chemical microanalysis

    DOEpatents

    Carr, M.J.; Romig, A.D. Jr.

    1987-08-05

    An x-ray mirror for both electron column instruments and micro x-ray fluorescence instruments for making chemical, microanalysis comprises a non-planar mirror having, for example, a spherical reflecting surface for x-rays comprised of a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on a substrate and whose layers have a thickness which is a multiple of the wavelength being reflected. For electron column instruments, the wavelengths of interest lie above 1.5nm, while for x-ray fluorescence instruments, the range of interest is below 0.2nm. 4 figs.

  12. Characterisation of mineralisation of bone and cartilage: X-ray diffraction and Ca and Sr K α X-ray fluorescence microscopy

    NASA Astrophysics Data System (ADS)

    Bradley, D. A.; Muthuvelu, P.; Ellis, R. E.; Green, E. M.; Attenburrow, D.; Barrett, R.; Arkill, K.; Colridge, D. B.; Winlove, C. P.

    2007-10-01

    Bone is a dynamic structure, constantly remodelling in response to changing mechanical and environmental factors. This is particularly evident in the mineral component encrusting the collagenous framework. The mineral is principally in the form of calcium apatite, but calcium can exchange with strontium, both during the cellular processes of mineralisation and resorption and by passive exchange with the deposited crystals. Mineralisation is generally characterized by densitometry, but because of the differences in absorption cross sections of calcium and strontium it can be misleading in studies of composition. In this work we have used X-ray diffraction to identify calcium and strontium apatite and X-ray fluorescence to quantify strontium and calcium distribution. With the beam characteristics available from synchrotron radiation, this has enabled us to obtain microscopic resolution on thin sections of bone and cartilage from the equine metacarpophalangeal joint. Two issues have been investigated; the first is the distribution of mineral in the bone-cartilage interface and within individual trabeculae. In trabecular bone the ratio of strontium to calcium concentration was typically 0.0035 ± 0.0020, and higher by a factor of ∼3 at the periphery than in the centre of a trabeculum (possibly reflecting the more rapid turnover of mineral in the surface layer). In the dense subchondral bone the ratio was similar, approximately doubling in the calcified cartilage. The second objective was to explore the changes in mineralisation associated with development of osteoarthrosis. We analysed lesions showing cartilage thinning and changes in the trabecular organization and density of the underlying bone. At the centre of the lesion the ratio of strontium to calcium was much lower than that in normal tissue, although the calcified cartilage still showed a higher ratio than the underlying bone. In the superficially normal tissue around the lesion the calcified cartilage

  13. Speciation and localization of Zn in the hyperaccumulator Sedum alfredii by extended X-ray absorption fine structure and micro-X-ray fluorescence.

    PubMed

    Lu, Lingli; Liao, Xingcheng; Labavitch, John; Yang, Xiaoe; Nelson, Erik; Du, Yonghua; Brown, Patrick H; Tian, Shengke

    2014-11-01

    Differences in metal homeostasis among related plant species can give important information of metal hyperaccumulation mechanisms. Speciation and distribution of Zn were investigated in a hyperaccumulating population of Sedum alfredii by using extended X-ray absorption fine structure and micro-synchrotron X-ray fluorescence (μ-XRF), respectively. The hyperaccumulator uses complexation with oxygen donor ligands for Zn storage in leaves and stems, and variations in the Zn speciation was noted in different tissues. The dominant chemical form of Zn in leaves was most probably a complex with malate, the most prevalent organic acid in S. alfredii leaves. In stems, Zn was mainly associated with malate and cell walls, while Zn-citrate and Zn-cell wall complexes dominated in the roots. Two-dimensional μ-XRF images revealed age-dependent differences in Zn localization in S. alfredii stems and leaves. In old leaves of S. alfredii, Zn was high in the midrib, margin regions and the petiole, whereas distribution of Zn was essentially uniform in young leaves. Zinc was preferentially sequestered by cells near vascular bundles in young stems, but was highly localized to vascular bundles and the outer cortex layer of old stems. The results suggest that tissue- and age-dependent variations of Zn speciation and distribution occurred in the hyperaccumulator S. alfredii, with most of the Zn complexed with malate in the leaves, but a shift to cell wall- and citric acid-Zn complexes during transportation and storage in stems and roots. This implies that biotransformation in Zn complexation occurred during transportation and storage processes in the plants of S. alfredii.

  14. Spatial distribution and speciation of arsenic in peat studied with Microfocused X-ray fluorescence spectrometry and X-ray absorption spectroscopy.

    PubMed

    Langner, Peggy; Mikutta, Christian; Suess, Elke; Marcus, Matthew A; Kretzschmar, Ruben

    2013-09-03

    Arsenic binding by sulfhydryl groups of natural organic matter (NOM) was recently identified as an important As sequestration pathway in the naturally As-enriched minerotrophic peatland Gola di Lago, Switzerland. Here, we explore the microscale distribution, elemental correlations, and chemical speciation of As in the Gola di Lago peat. Thin sections of undisturbed peat samples from 0-37 cm and 200-249 cm depth were analyzed by synchrotron microfocused X-ray fluorescence (μ-XRF) spectrometry and X-ray absorption spectroscopy (μ-XAS). Additionally, peat samples were studied by bulk As, Fe, and S K-edge XAS. Micro-XRF analyses showed that As in the near-surface peat was mainly concentrated in 10-50 μm sized hotspots, identified by μ-XAS as realgar (α-As4S4). In the deep peat layer samples, however, As was more diffusely distributed and mostly associated with particulate NOM of varying decomposition stages. The NOM-associated As was present as trivalent As bound by sulfhydryl groups. Arsenopyrite (FeAsS) and arsenian pyrite (FeAsxS2-x) of <25 μm size, which have escaped detection by bulk As and Fe K-edge XAS, were found as minor As species in the peat. Bulk S K-edge XAS revealed that the deep peat layers were significantly enriched in reduced organic S species. Our findings suggest an authigenic formation of realgar and arsenopyrite in strongly reducing microenvironments of the peat and indicate that As(III)-NOM complexes are formed by the passive sorption of As(III) to NOM. This reaction appears to be favored by a combination of abundant reduced organic S and comparatively low As solution concentrations preventing the formation of secondary As-bearing sulfides.

  15. Soft X-ray bremsstrahlung and fluorescent line production in the atmosphere by low energy electrons

    NASA Technical Reports Server (NTRS)

    Kraushaar, W. L.

    1974-01-01

    The effect of low energy quasi-trapped or precipitating electrons which impact on the counter windows of soft X-ray detectors are discussed. The errors caused by X-rays produced in the residual atmosphere above a rocket-borne detector because of the resemblance to X-rays of cosmic origin are examined. The design and development of counter windows which make it possible to identify the atmospherically produced X-rays are described. Curves are presented to show the following: (1) preliminary low energy electron data from Atmospheric Explorer C, (2) X-ray flux in electron-excited nitrogen and oxygen, (3) typical proportional counter response to low energy cosmic rays, and (4) proportional counter response to X-radiation produced by electrons incident upon a gas of oxygen to nitrogen number of 0.4.

  16. Iodine Vapor Staining for Atomic Number Contrast in Backscattered Electron and X-ray Imaging

    PubMed Central

    Boyde, Alan; Mccorkell, Fergus A; Taylor, Graham K; Bomphrey, Richard J; Doube, Michael

    2014-01-01

    Iodine imparts strong contrast to objects imaged with electrons and X-rays due to its high atomic number (53), and is widely used in liquid form as a microscopic stain and clinical contrast agent. We have developed a simple technique which exploits elemental iodine's sublimation-deposition state-change equilibrium to vapor stain specimens with iodine gas. Specimens are enclosed in a gas-tight container along with a small mass of solid I2. The bottle is left at ambient laboratory conditions while staining proceeds until empirically determined completion (typically days to weeks). We demonstrate the utility of iodine vapor staining by applying it to resin-embedded tissue blocks and whole locusts and imaging them with backscattered electron scanning electron microscopy (BSE SEM) or X-ray microtomography (XMT). Contrast is comparable to that achieved with liquid staining but without the consequent tissue shrinkage, stain pooling, or uneven coverage artefacts associated with immersing the specimen in iodine solutions. Unmineralized tissue histology can be read in BSE SEM images with good discrimination between tissue components. Organs within the locust head are readily distinguished in XMT images with particularly useful contrast in the chitin exoskeleton, muscle and nerves. Here, we have used iodine vapor staining for two imaging modalities in frequent use in our laboratories and on the specimen types with which we work. It is likely to be equally convenient for a wide range of specimens, and for other modalities which generate contrast from electron- and photon-sample interactions, such as transmission electron microscopy and light microscopy. Microsc. Res. Tech. 77:1044–1051, 2014. © 2014 The Authors. Microscopy Research Technique published by Wiley Periodocals, Inc. PMID:25219801

  17. Recent investigations of silk fibers utilizing x-ray scattering and atomic force microscopy

    NASA Astrophysics Data System (ADS)

    Miller, Lance D.

    1998-12-01

    Silks from the mulberry silkworm, Bombyx mori, and the golden-orb spider, Nephila clavipes, are materials that possess respectable properties. Even pitted against the high performance fibers of Kevlar, polyethylene, and carbon, the advantages of some of nature's fibers are clear. The tensile strength of the golden-orb spider dragline is of the same order of magnitude as many synthetic fibers, yet the dragline's compressive strength as a percentage of its tensile strength is greater. The spider's ampullate glands, responsible for the manufacture of the dragline, also excel. The spider spins its fiber from a liquid crystalline solution that is water based versus the solutions at high temperatures containing volatile solvents that are required for current synthetic fibers. Understanding the morphology of silks will provide the basis for improved manufacturing and better performing synthetic fibers. The studies presented here have centered on the use of small-angle x-ray scattering, SAXS, to describe the large-scale morphology of silk fibers. We have determined minimum scattering dimensions on the order of 150-300 nm. A detailed analysis of the Porod scattering region has revealed correlation lengths of the same magnitude. Both of these dimensions are similar to with direct atomic force microscopy, AFM, measurements of nanofibers found in samples of abraded or peeled silk. The incorporation of discrete Fourier transform theory and AFM topographic information has yielded results in general agreement with measured SAXS patterns. This incorporation allows the materials scientist a way of visualizing the relationship between a material and its resulting scattering function. We have also found that x-ray scattering gives insight to new periodic distances of the morphology of golden-orb dragline. All of these studies yield a more complete view of the silk morphology and give a new method of model building from scattering experiments.

  18. Comparing Compositions of Modern Cast Bronze Sculptures: Optical Emission Spectroscopy Versus x-Ray Fluorescence Spectroscopy

    NASA Astrophysics Data System (ADS)

    Young, M. L.; Dunand, D. C.

    2015-07-01

    Bulk elemental compositions of 74 modern cast bronze sculptures from the collection at the Art Institute of Chicago, the Philadelphia Museum of Art, and the Rodin Museum (Philadelphia, PA) were determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES) and a handheld x-ray fluorescence (XRF) spectrometer. The elemental compositions of the cast sculptures as measured previously by ICP-OES and presently by XRF are compared: A good match is found between the two methods for the base metal (Cu) and the two majority alloying elements (Zn and Sn). For both ICP-OES and XRF data, when the Zn composition is plotted versus the Sn composition, three discernable clusters are found that are related to the artist, foundry, casting date, and casting method; they consist of (A) high-zinc brass, (B) low-zinc, low-tin brass, and (C) low-zinc, tin bronze. Thus, our study confirms that the relatively fast, nondestructive XRF spectrometry can be used effectively over slower and invasive, but more accurate, ICP-OES to help determine a sculpture's artist, foundry, date of creation, date of casting, and casting method.

  19. [Research on the X-ray fluorescence spectrometry method to determine trace elements in kimberlite].

    PubMed

    Zhang, Lei; Yan, Chuan-wei; Lu, Yi

    2003-04-01

    It is very important to detect trace elements for kilmberlite. Through improving the working conditions of X-ray fluorescence spectrometer and optimizing the analytical conditions, the determination method of trace elements, such as Sc, Cr, Ni, Y, Nb, La, in kimberlite was worked out. The method has been successfully applied to the determination of trace elements in over 2 thousand samples of kimberlite from Liaoning province. The detection limits of the method were relatively low (the detection limit of Sc droped from 9.54 to 2.83 micrograms.g-1 and the detection limit of La droped from 21.68 micrograms.g-1 to 9.18 micrograms.g-1), i.e. 2.83, 2.15, 2.20, 1.17, 1.05 and 9.18 micrograms.g-1 for Sc, Cr, Ni, Y, Nb and La, respectively. The precision of the method was very high with 2.10%-7.09% of RSD (n = 20). Compared with ICP spectrometry this method is satisfactory. The method has proven to be simple and rapid with low cost and high efficiency.

  20. Elemental analysis of mining wastes by energy dispersive X-ray fluorescence (EDXRF)

    NASA Astrophysics Data System (ADS)

    Gonzalez-Fernandez, O.; Queralt, I.; Carvalho, M. L.; Garcia, G.

    2007-08-01

    An energy dispersive X-ray fluorescence (EDXRF) tri-axial geometry experimental spectrometer has been employed to determine the concentrations of 13 different elements (K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr and Pb) in mine wastes from different depths of two mine tailings from the Cartagena-La Union (Spain) mining district. The elements were determined and quantified using the fundamental parameters method. The concentrations of Cr, Ni, Cu, Zn and Pb were compared to the values from the European and Spanish legislation to evaluate the environmental risk and to classify the wastes as inert wastes or as wastes that have to be control land-filled. The results obtained demonstrate that these wastes can be considered as inert for the considered elements, apart from the concentration levels of Zn and Pb. Whilst Zn slightly overpasses the regulatory levels, Pb mean value exceeds three to six times the value to be considered as Class I potential land-filling material.

  1. The Distribution of Elements in 48 Canine Compact Bone Types Using Handheld X-Ray Fluorescence.

    PubMed

    Nganvongpanit, Korakot; Buddhachat, Kittisak; Piboon, Promporn; Klinhom, Sarisa

    2016-11-01

    A major question when we talk about the elements in the bone is whether all bones contain the same elements. To answer this question, this study was designed for determination of the elemental levels in 48 various canine compact bones using handheld X-ray fluorescence technique. From a total of 26 elements that could be detected, only 13 elements were found in all 48 bones. The sternum and os penis were significantly different from the other bones in that they contained the highest number of elements. The ratio of Ca and P was significantly different when comparing certain bones: there was a higher Ca/P ratio in the patella (right), calcaneus (right and left), and sternum compared with a lower ratio in the radius (left), rib (left), phalanx (left forelimb), and carpus (left). These results are the first to demonstrate that different types of bones have different elemental profiles, even for major elements such as Ca and P. Moreover, the Ca/P ratio was also different between bone types. This data is important for the selection of bones appropriate to the element studied. In addition, the results proved that the elements were not equally distributed in every bone in the body.

  2. Green direct determination of mineral elements in artichokes by infrared spectroscopy and X-ray fluorescence.

    PubMed

    Mir-Marqués, Alba; Martínez-García, Maria; Garrigues, Salvador; Cervera, M Luisa; de la Guardia, Miguel

    2016-04-01

    Near infrared (NIR) and X-ray fluorescence (XRF) spectroscopy were investigated to predict the concentration of calcium, potassium, iron, magnesium, manganese and zinc in artichoke samples. Sixty artichokes were purchased from different Spanish areas (Benicarló, Valencia and Murcia). NIR and XRF spectra, combined with partial least squares (PLS) data treatment, were used to develop chemometric models for the prediction of mineral concentration. To obtain reference data, samples were mineralised and analysed by inductively coupled plasma optical emission spectrometry (ICP-OES). Coefficients of determination obtained for the regression between predicted values and reference ones for calcium, potassium, magnesium, iron, manganese and zinc were 0.61, 0.79, 0.53, 0.77, 0.54 and 0.60 for NIR and 0.96, 0.93, 0.80, 0.79, 0.76 and 0.90 for XRF, respectively. Both assayed methodologies, offer green alternatives to classical mineral analysis, but XRF provided the best results in order to be used as a quantitative screening method.

  3. Comparison of gold leaf thickness in Namban folding screens using X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Pessanha, Sofia; Madeira, Teresa I.; Manso, Marta; Guerra, Mauro; Le Gac, Agnès; Carvalho, Maria Luisa

    2014-09-01

    In this work, the thickness of the gold leaf applied in six Japanese folding screens is compared using a nondestructive approach. Four screens belonging to the Momoyama period (~1573-1603) and two screens belonging to the early Edo period (~1603-1868) were analyzed in situ using energy dispersive X-ray fluorescence, and the thickness of the applied gold leaf was evaluated using a methodology based on the attenuation of the different characteristic lines of gold in the gold leaf layer. Considering that the leaf may well not be made of pure gold, we established that, for the purpose of comparing the intensity ratios of the Au lines, layers made with gold leaf of high grade can be considered identical. The gold leaf applied in one of the screens from the Edo period was found to be thinner than the gold leaf applied in the other ones. This is consistent with the development of the beating technology to obtain ever more thin gold leafs.

  4. X-ray fluorescence microscopy reveals the role of selenium in spermatogenesis.

    PubMed

    Kehr, Sebastian; Malinouski, Mikalai; Finney, Lydia; Vogt, Stefan; Labunskyy, Vyacheslav M; Kasaikina, Marina V; Carlson, Bradley A; Zhou, You; Hatfield, Dolph L; Gladyshev, Vadim N

    2009-06-26

    Selenium (Se) is a trace element with important roles in human health. Several selenoproteins have essential functions in development. However, the cellular and tissue distribution of Se remains largely unknown because of the lack of analytical techniques that image this element with sufficient sensitivity and resolution. Herein, we report that X-ray fluorescence microscopy (XFM) can be used to visualize and quantify the tissue, cellular, and subcellular topography of Se. We applied this technique to characterize the role of Se in spermatogenesis and identified a dramatic Se enrichment specifically in late spermatids, a pattern that was not seen in any other elemental maps. This enrichment was due to elevated levels of the mitochondrial form of glutathione peroxidase 4 and was fully dependent on the supplies of Se by selenoprotein P. High-resolution scans revealed that Se concentrated near the lumen side of elongating spermatids, where structural components of sperm are formed. During spermatogenesis, maximal Se associated with decreased phosphorus, whereas Zn did not change. In sperm, Se was primarily in the midpiece and colocalized with Cu and Fe. XFM allowed quantification of Se in the midpiece (0.8 fg) and head (0.2 fg) of individual sperm cells, revealing the ability of sperm cells to handle the amounts of this element well above its toxic levels. Overall, the use of XFM allowed visualization of tissue and cellular Se and provided important insights in the role of this and other trace elements in spermatogenesis.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. Micro energy-dispersive x-ray fluorescence spectrometry study of dentin coating with nanobiomaterials

    NASA Astrophysics Data System (ADS)

    Soares, Luís. Eduardo Silva; Nahorny, Sídnei; Marciano, Fernanda Roberta; Zanin, Hudson; Lobo, Anderson de Oliveira

    2015-06-01

    New biomaterials such as multi-walled carbon nanotubes oxide/graphene oxide (MWCNTO/GO), nanohydroxyapatite (nHAp) and combination of them together or not to acidulated phosphate fluoride gel (F) have been tested as protective coating before root dentin erosion. Fourteen bovine teeth were cleaned, polished, divided into two parts (n=28) and assigned to seven groups: (Control) - without previous surface treatment; F treatment; nHAp; MWCNTO/GO; F+nHAp; F+MWCNTO/GO and F+MWCNTO/GO/nHAp composites. Each sample had two sites of pre-treatments: acid etched area and an area without treatment. After the biomaterials application, the samples were submitted to six cycles (demineralization: orange juice, 10 min; remineralization: artificial saliva, 1 h). Micro energy-dispersive X-ray fluorescence spectrometry (μ-EDXRF) mapping area analyses were performed after erosive cycling on both sites (n=84). μ-EDXRF mappings showed that artificial saliva and MWCNTO/GO/nHAp/F composite treatments produced lower dentin demineralization than in the other groups. Exposed dentin tubules allowed better interaction of nanobiomaterials than in smear layer covered dentin. Association of fluoride with other biomaterials had a positive influence on acid etched dentin. MWCNTO/GO/nHAp/F composite treatment resulted in levels of demineralization similar to the control group.

  7. Optimal configuration for detection of gold nanoparticles in tumors using Kβ X-ray fluorescence line

    NASA Astrophysics Data System (ADS)

    Figueroa, R. G.; Santibañez, M.; Malano, F.; Valente, M.

    2015-12-01

    This study examines the increase in the capacity to detect gold nanoparticles in tumor tissue using X-rays from orthovoltage sources. The analyzed methodology considered aspects of geometry and composition in accordance with those required in real clinical treatment applications. The results show that a geometrical backscatter configuration, an incident spectral energy synthesized to optimize statistical parameters and adequate background subtraction allow for a significant increase in the signal to noise ratio (SNR) of the secondary Kβ lines. This increase is greater than those currently reported for traditional Kα lines. Furthermore, these conditions also produce an increase in detection sensitivity, less uncertainty in results and shorter exposure times. The proposed methodology was evaluated using XMI-MSIM software for the Monte Carlo simulation fluorescent response of each element. The simulation used tumors of 1-3 cm3, at a depth of 1-5 cm with a 0.1-1% gold nanoparticle concentration. The measurement time and the skin entrance dose by the methodology were considered for allows future quantitative surface scanning implementation.

  8. Rainwater analysis by synchrotron radiation-total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    López, María L.; Ceppi, Sergio A.; Asar, María L.; Bürgesser, Rodrigo E.; Ávila, Eldo E.

    2015-11-01

    Total reflection X-ray fluorescence analysis excited with synchrotron radiation was used to quantify the elemental concentration of rainwater in Córdoba, Argentina. Standard solutions with gallium as internal standard were prepared for the calibration curves. Rainwater samples of 5 μl were added to an acrylic reflector, allowed to dry, and analyzed for 200 s measuring time. The elemental concentrations of As, Ca, Co, Cr, Cu, Fe, K, Mn, Ni, Pb, S, Sr, V, and Zn were determined. The electrical conductivity, pH, and elemental concentrations were compared to data previously reported for the soluble fraction of rainwater at different sites. A factor analysis was performed in order to determine the sources that contributed to the elemental concentration in rainwater. Anthropogenic sources were identified as traffic pollution, vehicular emissions, and metallurgical factories. The quality of rainwater was analyzed by comparing the concentrations of all the elements in rainwater samples with the WHO guideline values for drinking water. The results show the need to control the atmospheric emissions in order to preserve the quality of rainwater. SR-TXRF analysis of chemical composition of rainwater in Córdoba represents the very first contribution in the region to the knowledge of the concentration of trace metals in the soluble fraction of rainwater. These data are scarce, especially in the Southern Hemisphere.

  9. Algorithms for a hand-held miniature x-ray fluorescence analytical instrument

    SciTech Connect

    Elam, W.T.; Newman, D.; Ziemba, F.

    1998-12-31

    The purpose of this joint program was to provide technical assistance with the development of a Miniature X-ray Fluorescence (XRF) Analytical Instrument. This new XRF instrument is designed to overcome the weaknesses of spectrometers commercially available at the present time. Currently available XRF spectrometers (for a complete list see reference 1) convert spectral information to sample composition using the influence coefficients technique or the fundamental parameters method. They require either a standard sample with composition relatively close to the unknown or a detailed knowledge of the sample matrix. They also require a highly-trained operator and the results often depend on the capabilities of the operator. In addition, almost all existing field-portable, hand-held instruments use radioactive sources for excitation. Regulatory limits on such sources restrict them such that they can only provide relatively weak excitation. This limits all current hand-held XRF instruments to poor detection limits and/or long data collection times, in addition to the licensing requirements and disposal problems for radioactive sources. The new XRF instrument was developed jointly by Quantrad Sensor, Inc., the Naval Research Laboratory (NRL), and the Department of Energy (DOE). This report describes the analysis algorithms developed by NRL for the new instrument and the software which embodies them.

  10. Total reflection X-ray fluorescence as a fast multielemental technique for human placenta sample analysis

    NASA Astrophysics Data System (ADS)

    Marguí, E.; Ricketts, P.; Fletcher, H.; Karydas, A. G.; Migliori, A.; Leani, J. J.; Hidalgo, M.; Queralt, I.; Voutchkov, M.

    2017-04-01

    In the present contribution, benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been evaluated as a cost-effective multielemental analytical technique for human placenta analysis. An easy and rapid sample preparation consisting of suspending 50 mg of sample in 1 mL of a Triton 1% solution in deionized water showed to be the most suitable for this kind of samples. However, for comparison purposes, an acidic microwave acidic digestion procedure was also applied. For both sample treatment methodologies, limits of detection for most elements were in the low mg/kg level. Accurate and precise results were obtained using internal standardization as quantification approach and applying a correction factor to compensate for absorption effects. The correction factor was based on the proportional ratio between the slurry preparation results and those obtained for the analysis of a set of human placenta samples analysed by microwave acidic digestion and ICP-AES analysis. As a study case, the developed TXRF methodology was applied for multielemental analysis (K, Ca, Fe, Cu, Zn, As, Se, Br, Rb and Sr) of several healthy women's placenta samples from two regions in Jamaica.

  11. Imaging of stroke: a comparison between X-ray fluorescence and magnetic resonance imaging methods.

    PubMed

    Zheng, Weili; Haacke, E Mark; Webb, Samuel M; Nichol, Helen

    2012-12-01

    A dual imaging approach, combining magnetic resonance imaging to localize lesions and synchrotron rapid scanning X-ray fluorescence (XRF) mapping to localize and quantify calcium, iron and zinc was used to examine one case of recent stroke with hemorrhage and two cases of ischemia 3 and 7 years before death with the latter showing superficial necrosis. In hemorrhagic lesions, more Fe is found accompanied with less Zn. In chronic ischemic lesions, Fe, Zn and Ca are lower indicating that these elements are removed as the normal tissue dies and scar tissue forms. Both susceptibility and T2* maps were calculated to visualize iron in hemorrhages and validated by XRF Ca and Fe maps. The former was superior for imaging iron in hemorrhagic transformation and necrosis but did not capture ischemic lesions. In contrast, T2* could not differentiate Ca from Fe in necrotic tissue but did capture ischemic lesions, complementing the susceptibility mapping. The spatial localization, accurate quantitative data and elemental differentiation shown here could also be valuable for imaging other brain tissue damage with abnormal Ca and Fe content.

  12. X-ray Fluorescence Spectroscopy Study of Coating Thickness and Base Metal Composition

    NASA Technical Reports Server (NTRS)

    Rolin, T. D.; Leszczuk, Y.

    2008-01-01

    For electrical, electronic, and electromechanical (EEE) parts to be approved for space use, they must be able to meet safety standards approved by NASA. A fast, reliable, and precise method is needed to make sure these standards are met. Many EEE parts are coated in gold (Au) and nickel (Ni), and the thickness coating is crucial to a part s performance. A nondestructive method that is efficient in measuring coating thickness is x-ray fluorescence (XRF) spectroscopy. The XRF spectrometer is a machine designed to measure layer thickness and composition of single or multilayered samples. By understanding the limitations in the collection of the data by this method, accurate composition and thickness measurements can be obtained for samples with Au and Ni coatings. To understand the limitations of data found, measurements were taken with the XRF spectrometer and compared to true values of standard reference materials (SRM) that were National Institute of Standards and Technology (NIST) traceable. For every sample, six different parameters were varied to understand measurement error: coating/substrate combination, number of layers, counting interval, collimator size, coating thickness, and test area location. Each measurement was taken in accordance with standards set by the American Society for Testing and Materials (ASTM) International Standard B 568.

  13. Non-destructive investigation of a time capsule using neutron radiography and X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    MacDonald, B. L.; Vanderstelt, J.; O'Meara, J.; McNeill, F. E.

    2016-01-01

    Non-destructive analytical techniques are becoming increasingly important for the study of objects of cultural heritage interest. This study applied two techniques: X-ray fluorescence and neutron radiography, for the investigation of a capped, tubular metal object recovered from an urban construction site in Gore Park, Hamilton, Canada. The site is an urban park containing a World War I commemorative monument that underwent renovation and relocation. Historical documentation suggested that the object buried underneath the monument was a time capsule containing a paper document listing the names of 1800 Canadians who died during WWI. The purpose of this study was to assess the condition of the object, and to verify if it was what the historical records purported. XRF analysis was used to characterize the elemental composition of the metal artifact, while neutron radiography revealed that its contents were congruent with historical records and remained intact after being interred for 91 years. Results of this study demonstrate the value of non-destructive techniques for the analysis and preservation of cultural heritage.

  14. Using Synchrotron X-ray Fluorescence Microprobes in the Study of Metal Homeostasis in Plants

    SciTech Connect

    Punshon, T.; Guerinot, M; Lanzirotti, A

    2009-01-01

    Background and Aims: This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope: The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions: SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis.

  15. [X-ray fluorescence spectrum studies on bioorganic carbon in cereals and carbon chemical circulation].

    PubMed

    Duan, De-liang; Bian, Fu-yong; Yuan, Bo; Wang, Shu; Ge, Mao-fa; Zhang, Xing-kang; Xu, Si-chuan

    2011-05-01

    The bioorganic carbon contents and chemical element compositions in six kinds of cereals: paddy (rice), wheat (flour), soybean, millet, sorghum and corn were determined by X-ray fluorescence (XRF) spectrum, meanwhile a new method was established to probe their protein contents. In the cereals, the average bioorganic carbon content is about 440%. The highest protein content is 42.74% from soybean, and other protein content is 28.56% in millet, 27.57% in wheat, 24.99% in corn, 22.21% in sorghum, but only 20.31% in rice. Based on our new definition of carbon chemical circulation presented in the current work, the authors have found that in 2009 humankind used bioorganic carbon to discharge CO2 into the earth's atmosphere that accounts for one percent of the total CO2 discharge, and consumed organic carbon to release CO2 into the earth's atmosphere, accounting for 10.73% of the total CO2 discharge. The clear definition of carbon chemical circulation and the discharged CO2 content from the distinct types of carbon compounds would advance the study on carbon chemical circulation and the atmospheric CO2 greenhouse effect. Our work further found that it takes eight years to circulate the total earth's atmospheric CO2. The short period shows the sensitivity for CO2 to keep its dynamical equilibrium in the earth's atmosphere. However, no experimental data has been reported to prove a heavy destructive greenhouse effect of CO2 existing in the earth's atmosphere.

  16. Synchrotron X-ray fluorescence spectroscopy of salts in natural sea ice

    NASA Astrophysics Data System (ADS)

    Obbard, Rachel W.; Lieb-Lappen, Ross M.; Nordick, Katherine V.; Golden, Ellyn J.; Leonard, Jeremiah R.; Lanzirotti, Antonio; Newville, Mathew G.

    2016-11-01

    We describe the use of synchrotron-based X-ray fluorescence spectroscopy to examine the microstructural location of specific elements, primarily salts, in sea ice. This work was part of an investigation of the location of bromine in the sea ice-snowpack-blowing snow system, where it plays a part in the heterogeneous chemistry that contributes to tropospheric ozone depletion episodes. We analyzed samples at beamline 13-ID-E of the Advanced Photon Source at Argonne National Laboratory. Using an 18 keV incident energy beam, we produced elemental maps of salts for sea ice samples from the Ross Sea, Antarctica. The distribution of salts in sea ice depends on ice type. In our columnar ice samples, Br was located in parallel lines spaced roughly 0.5 mm apart, corresponding to the spacing of lamellae in the skeletal region during initial ice growth. The maps revealed concentrations of Br in linear features in samples from all but the topmost and bottommost depths. For those samples, the maps revealed rounded features. Calibration of the Br elemental maps showed bulk concentrations to be 5-10 g/m3, with concentrations ten times larger in the linear features. Through comparison with horizontal thin sections, we could verify that these linear features were brine sheets or layers.

  17. X-ray fluorescence spectroscopy and Monte Carlo characterization of a unique nuragic artifact (Sardinia, Italy)

    NASA Astrophysics Data System (ADS)

    Brunetti, Antonio; Depalmas, Anna; di Gennaro, Francesco; Serges, Alessandra; Schiavon, Nicola

    2016-07-01

    The chemical composition of a unique bronze artifact known as the "Cesta" ("Basket") belonging to the ancient Nuragic civilization of the Island of Sardinia, Italy has been analyzed by combining X-ray Fluorescence Spectroscopy (XRF) with Monte Carlo simulations using the XRMC code. The "Cesta" had been discovered probably in the XVIII century with the first graphic representation reported around 1761. In a later draft (dated 1764), the basket has been depicted as being carried upside-down on the shoulder of a large bronze warrior Barthélemy (1761), Pinza (1901), Winckelmann (1776) . The two pictorial representations differed only by the presence of handles in the most recent one. XRF measurements revealed that the handles of the object are composed by brass while the other parts are composed by bronze suggesting the handles as being a later addition to the original object. The artifact is covered at its surface by a fairly thick corrosion patina. In order to determine the bronze bulk composition without the need for removing the outer patina, the artifact has been modeled as a two layer object in Monte Carlo simulations.

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

    NASA Astrophysics Data System (ADS)

    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.

  19. HIGH RESOLUTION X-RAY FLUORESCENCE MICRO-TOMOGRAPHY ON SINGLE SEDIMENT PARTICLES.

    SciTech Connect

    VINCZE,L.; VEKEMANS,B.; SZALOKI,I.; JANSSENS,K.; VAN GRIEKEN,R.; FENG,H.; JONES,K.W.; ADAMS,F.

    2002-07-29

    This work focuses on the investigation of the distribution of contaminants in individual sediment particles from the New York/New Jersey Harbor. Knowledge of the spatial distribution of the contaminants within the particles is needed to enable (1) more sophisticated approaches to the understanding of the fate and transport of the contaminants in the environment and (2) more refined methods for cleaning the sediments. The size of the investigated particles ranges from 30-80 microns. Due to the low concentration of the elements of interest and the microscopic size of the environmental particles in these measurements, the small size and high intensity of the analyzing X-ray beam was critical. The high photon flux at the ESRF Microfocus beam line (ID13) was used as the basis for fluorescence tomography to investigate whether the inorganic compounds are taken upon the surface organic coating or whether they are distributed through the volume of the grains being analyzed. The experiments were done using a 13 keV monochromatic beam of approximately 2 {micro}m in size having an intensity of 10{sup 10} ph/s, allowing absolute detection limits on the 0.04-1 fg level for Ti, Cr, Mn, Fe, Ni, and Zn.

  20. Determination of element levels in human serum: Total reflection X-ray fluorescence applications

    NASA Astrophysics Data System (ADS)

    Majewska, U.; Łyżwa, P.; Łyżwa, K.; Banaś, D.; Kubala-Kukuś, A.; Wudarczyk-Moćko, J.; Stabrawa, I.; Braziewicz, J.; Pajek, M.; Antczak, G.; Borkowska, B.; Góźdź, S.

    2016-08-01

    Deficiency or excess of elements could disrupt proper functioning of the human body and could lead to several disorders. Determination of their concentrations in different biological human fluids and tissues should become a routine practice in medical treatment. Therefore the knowledge about appropriate element concentrations in human organism is required. The purpose of this study was to determine the concentration of several elements (P, S, Cl, K, Ca, Cr, Fe, Cu, Zn, Se, Br, Rb, Pb) in human serum and to define the reference values of element concentration. Samples of serum were obtained from 105 normal presumably healthy volunteers (66 women aged between 15 and 78 years old; 39 men aged between 15 and 77 years old). Analysis has been done for the whole studied population and for subgroups by sex and age. It is probably first so a wide study of elemental composition of serum performed in the case of Świętokrzyskie region. Total reflection X-ray fluorescence (TXRF) method was used to perform the elemental analysis. Spectrometer S2 Picofox (Bruker AXS Microanalysis GmbH) was used to identify and measure elemental composition of serum samples. Finally, 1st and 3rd quartiles were accepted as minimum and maximum values of concentration reference range.