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Sample records for 3d-micro x-ray fluorescence

  1. Methodology toward 3D micro X-ray fluorescence imaging using an energy dispersive charge-coupled device detector.

    Garrevoet, Jan; Vekemans, Bart; Tack, Pieter; De Samber, Björn; Schmitz, Sylvia; Brenker, Frank E; Falkenberg, Gerald; Vincze, Laszlo

    2014-12-01

    A new three-dimensional (3D) micro X-ray fluorescence (μXRF) methodology based on a novel 2D energy dispersive CCD detector has been developed and evaluated at the P06 beamline of the Petra-III storage ring (DESY) in Hamburg, Germany. This method is based on the illumination of the investigated sample cross-section by a horizontally focused beam (vertical sheet beam) while fluorescent X-rays are detected perpendicularly to the sheet beam by a 2D energy dispersive (ED) CCD detector allowing the collection of 2D cross-sectional elemental images of a certain depth within the sample, limited only by signal self-absorption effects. 3D elemental information is obtained by a linear scan of the sample in the horizontal direction across the vertically oriented sheet beam and combining the detected cross-sectional images into a 3D elemental distribution data set. Results of the 3D μXRF analysis of mineral inclusions in natural deep Earth diamonds are presented to illustrate this new methodology. PMID:25346101

  2. Chemical U-Th-Pb dating of monazite by 3D-Micro x-ray fluorescence analysis with synchrotron radiation

    Schmitz, Susanne; Möller, Andreas; Wilke, Max;

    2009-01-01

    A confocal set-up for three-dimensional (3D) micro X-ray fluorescence (micro-XRF) was used at the mySpot beamline at BESSY II, which allows compositional depth profiling for various applications. We present results obtained with a confocal 3D micro-XRF set-up for chemical age dating using the U, Th...... and Pb concentrations of monazite within rock thin sections. The probing volume was determined to be approximately 21 × 21 × 24 µm3 for W-La using an excitation energy of 19 keV. The relative detection limits particularly for Pb are below 10 ppm (for counting times of 1000 s). Therefore, this 3D micro-XRF...... ages, varying from 20 Ma to 1.82 Ga. Reference materials (GM3, F6, 3345) can be reproduced within error. The spread in the ages of all points determined by 3D micro-XRF is within 8 % of the isotopic reference value. The average 3D micro-XRF dates reproduce the reference ages with discrepancies between...

  3. X-ray Fluorescence Sectioning

    Cong, Wenxiang

    2012-01-01

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

  4. X-ray fluorescence holography

    Hayashi, K; Takahashi, Y

    2003-01-01

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

  5. X-ray fluorescence spectrometry

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

  6. Detection limits in x-ray fluorescence analysis

    X-ray fluorescence spectrometry is a well established analytical technique for elemental analysis of solids, powders, or liquids. This extended abstract briefly discusses the detection limits or sensitivity of x-ray spectrometers in x-ray fluorescence analysis

  7. Simulation of x-ray fluorescence spectra

    A method for simulating x-ray fluorescence (XRF) spectra in hybrid densitometry is presented. This technique allows simulation of XRF spectra for solutions with arbitrary concentrations of special nuclear material and minor actinides excited by an x-ray generator. Spectra for mixed uranium and plutonium solutions with U/Pu ratios ranging from 100 to 1 have been generated. This range of ratios applies to most solutions found in plutonium reprocessing plants. XRF simulation can provide important data for estimating instrument precision, evaluating analysis techniques, and training system operators. Applications of XRF simulation in the development of the Los Alamos Hybrid K-Edge/XRF Densitometer system are described

  8. Development of confocal micro X-ray fluorescence instrument using two X-ray beams

    A new confocal micro X-ray fluorescence instrument was developed. This instrument has two independent micro X-ray tubes with Mo targets. A full polycapillary X-ray lens was attached to each X-ray tube. Another half polycapillary lens was attached to a silicon drift X-ray detector (SDD). The focal spots of the three lenses were adjusted to a common position. The effects of the excitation of two X-ray beams were investigated. The instrument enabled highly sensitive three-dimensional X-ray fluorescence analysis. We confirmed that the X-ray fluorescence intensity from the sample increased by applying the two independent X-ray tubes in confocal configuration. Elemental depth profiling of black wheat was demonstrated with the result that each element in the surface coat of a wheat grain showed unique distribution

  9. First X-ray fluorescence CT experimental results at the SSRF X-ray imaging beamline

    DENG Biao; YANG Qun; XIE Hong-Lan; DU Guo-Hao; XIAO Wi-Qiao

    2011-01-01

    X-ray fluorescence CT is a non-destructive technique for detecting elemental composition and distribution inside a specimen. In this paper, the first experimental results of X-ray fluorescence CT obtained at the SSRF X-ray imaging beamline (BL13W1) are described. The test samples were investigated and the 2D elemental image was reconstructed using a filtered back-projection algorithm. In the sample the element Cd was observed. Up to now, the X-ray fluorescence CT could be carried out at the SSRF X-ray imaging beamline.

  10. Surface-Enhanced X-Ray Fluorescence

    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.

  11. Silicon lithium detector for x ray fluorescence

    The Silicon Lithium detector is the system for the detection of nuclear radiation. It transforms the charge that was produced inside of Silicon material as a result of the incidence of particles and X rays, in voltage pulses at the output of the preamplifier. In this work was made the adjustment of the technological process of manufacture of the detector. Also was made the design and construction of the cryostat and preamplifier and then the validation of the system in a Cuban Dewar. The system, which was made for the first time in our country, has an energy resolution of 185 eV for the Fe-55 source (E=5.9 KeV), which has permitted its implementation in energy dispersive X ray fluorescence. (author)

  12. Total reflection X-ray fluorescence analysis

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

  13. In vivo X-ray fluorescence analysis

    Measurements on five occupationally exposed persons have shown that it is possible to use X-ray fluorescence analysis for in vivo measurements of lead in the skeleton. The technique for calibrating in vivo X-ray fluorescence measurements of lead in bone tissue has been studied in detail and a two-component phantom simulating the bone and the soft tissue parts of the finger constructed. The technique has been used for in vivo measurements on 22 occupationally exposed persons. The minimum detectable concentration of lead in fingerbones was found to be around 20 μg x g-1. The lead concentrations in their skeletons and blood were compared: the correlation was poor. The variations in lead concentrations in the skeleton have been studied in occupationally exposed persons and in samples from archaeological skeletons. The sensitivity and the minimum detectable concentration of cadmium in the kidney cortex in in vivo measurements has been studied by measurements on kidney models. The minimum detectable concentration was 20 μg x g-1 at a skin-kidney distance of 30 mm and 40 μg x g-1 at 40 mm. Five persons occupationally exposed were studied. (Author)

  14. Laser-based X-ray and electron source for X-ray fluorescence studies

    Valle Brozas, F.; Crego, A.; Roso, L.; Peralta Conde, A.

    2016-08-01

    In this work, we present a modification to conventional X-rays fluorescence using electrons as excitation source and compare it with the traditional X-ray excitation for the study of pigments. For this purpose, we have constructed a laser-based source capable to produce X-rays as well as electrons. Because of the large penetration depth of X-rays, the collected fluorescence signal is a combination of several material layers of the artwork under study. However, electrons are stopped in the first layers, allowing a more superficial analysis. We show that the combination of both excitation sources can provide extremely valuable information about the structure of the artwork.

  15. Fluorescence X-ray micro-spectroscopy activities at ESRF

    Salome, M; Bleuet, P; Chalmin, E; Cloetens, P; Andrade, V De; Martinez-Criado, G; Petitgirard, S; Rak, M; Tresserras, J A Sans; Tucoulou, R; Susini, J [European Synchrotron Radiation Facility, X-ray Imaging Group, BP 220, F-38043 Grenoble Cedex (France); Bohic, S [INSERM U-836, Institut des Neurosciences Grenoble, Universite Joseph Fourier UMR-S 836, F-38042 Grenoble (France); Cauzid, J [CREGU and UMR G2R 7566, Universite Poincare, BP 23, F-54506 Vandoeuvre-Les-Nancy Cedex (France); Cotte, M [Centre de Recherche et de Restauration des Musees de France, CNRS-UMR 171, Palais du Louvre, 14, quai Francois Mitterrand, F-7501 Paris (France); Szlachetko, J, E-mail: salome@esrf.f [Institute of Physics, Jan Kochanowski University, 25-406 Kielce (Poland)

    2009-09-01

    The X-ray Microscopy and Micro-analysis beamlines at ESRF operate complementary state-of-the-art instruments at ID21, ID22, ID18F and more recently ID22NI. Within a multi-modal strategy, these beamlines develop micro-imaging techniques with various contrast mechanisms ({mu}XRF, {mu}XANES, {mu}XRD and phase contrast) and host experiments with scientific topics ranging from Geochemistry to Archeology, Environmental sciences, Biology and Material sciences. Future challenges include pushing spatial resolution down to the nano-scale and the development of innovative 3D micro-analysis techniques.

  16. X-ray fluorescence micro-tomography and laminography using an x-ray scanning microscope

    Watanabe, N.; Hoshino, M.; Yamamoto, K.; Aoki, S.; Takeuchi, A.; Suzuki, Y.

    2009-09-01

    Using a scanning microscope with a zone plate, x-ray fluorescence micro-tomography was investigated at SPring-8 BL20XU. A 120 nm-thick zinc layer could be resolved in the reconstructed section image. A frozen phytoplankton and a iron impurity of a diamond could be also reconstructed. X-ray fluorescence laminography was tested at SPring-8 BL47XU. A tantalum line pattern of 3 μm line width could be reconstructed.

  17. X-ray fluorescence micro-tomography and laminography using an x-ray scanning microscope

    Watanabe, N; Hoshino, M; Yamamoto, K; Aoki, S [Institute of Applied Physics, University of Tsukuba, Tsukuba, Ibaraki 305-8573 (Japan); Takeuchi, A; Suzuki, Y, E-mail: watanabe@bk.tsukuba.ac.j [SPring-8, JASRI, Mikazuki, Hyogo 679-5198 (Japan)

    2009-09-01

    Using a scanning microscope with a zone plate, x-ray fluorescence micro-tomography was investigated at SPring-8 BL20XU. A 120 nm-thick zinc layer could be resolved in the reconstructed section image. A frozen phytoplankton and a iron impurity of a diamond could be also reconstructed. X-ray fluorescence laminography was tested at SPring-8 BL47XU. A tantalum line pattern of 3 {mu}m line width could be reconstructed.

  18. X-ray fluorescence micro-tomography and laminography using an x-ray scanning microscope

    Using a scanning microscope with a zone plate, x-ray fluorescence micro-tomography was investigated at SPring-8 BL20XU. A 120 nm-thick zinc layer could be resolved in the reconstructed section image. A frozen phytoplankton and a iron impurity of a diamond could be also reconstructed. X-ray fluorescence laminography was tested at SPring-8 BL47XU. A tantalum line pattern of 3 μm line width could be reconstructed.

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

    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.

  20. Advanced of X-ray fluorescence logging technique in China

    The paper discuses principle of X-ray fluorescence logging, and introduces advanced of X-ray fluorescence logging technique in China. By 2009, third generation XRF logging instrument has been developed in China, and good logging result has been obtained in Lala copper mine. (authors)

  1. Laser-based X-ray and electron source for X-ray fluorescence studies

    Brozas, F Valle; Roso, L; Conde, A Peralta

    2016-01-01

    In this work we present a modification to conventional X-rays fluorescence using electrons as excitation source, and compare it with the traditional X-ray excitation for the study of pigments. For this purpose we have constructed a laser-based source capable to produce X-rays as well as electrons. Because of the large penetration depth of X-rays, the collected fluorescence signal is a combination of several material layers of the artwork under study. However electrons are stopped in the first layers allowing therefore a more superficial analysis. We show that the combination of both excitation sources can provide extremely valuable information about the structure of the artwork.

  2. Energy-dispersive X-ray diffraction mapping on a benchtop X-ray fluorescence system

    Lane, DW; Nyombi, A; Shackel, J

    2014-01-01

    A method for energy-dispersive X-ray diffraction mapping is presented, using a conventional low-power benchtop X-ray fluorescence spectrometer, the Seiko Instruments SEA6000VX. Hyper spectral X-ray maps with a 10µm step size were collected from polished metal surfaces, sectioned Bi, Pb and steel shot gun pellets. Candidate diffraction lines were identified by eliminating those that matched a characteristic line for an element and those predicted for escape peaks, sum peaks, and Rayleigh and C...

  3. X-ray fluorescence in investigations of archaeological finds

    Cechak, T. [Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, Brehova 7, 115 19 Prague 1 (Czech Republic); Hlozek, M. [Institute of Archaeology and Museology, Masaryk University, Arna Novaka 1, 602 00 Brno (Czech Republic); Musilek, L. [Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, Brehova 7, 115 19 Prague 1 (Czech Republic)], E-mail: musilek@fjfi.cvut.cz; Trojek, T. [Faculty of Nuclear Sciences and Physical Engineering, Czech Technical University in Prague, Brehova 7, 115 19 Prague 1 (Czech Republic)

    2007-10-15

    X-ray fluorescence can be successfully used for analysing the elemental composition of the superficial layers of a measured object, especially for investigating surface coatings, deposits of adventitious materials on the surface, etc. An energy dispersive version of X-ray fluorescence analysis is used in our investigations for analysing various historic objects, art works and archaeological finds. Examples of the application of X-ray fluorescence to various archaeological finds from excavations in the Czech Republic are presented - shards of ancient glazed ceramics, moulds for casting metal products, the remains of a human finger with traces of brass, probably from a ring, etc.

  4. X-ray fluorescence in investigations of archaeological finds

    X-ray fluorescence can be successfully used for analysing the elemental composition of the superficial layers of a measured object, especially for investigating surface coatings, deposits of adventitious materials on the surface, etc. An energy dispersive version of X-ray fluorescence analysis is used in our investigations for analysing various historic objects, art works and archaeological finds. Examples of the application of X-ray fluorescence to various archaeological finds from excavations in the Czech Republic are presented - shards of ancient glazed ceramics, moulds for casting metal products, the remains of a human finger with traces of brass, probably from a ring, etc

  5. Research in quantitative microscopic X-ray fluorescence analysis

    A feasibility study of quantitative elemental microanalysis of biological materials and glass samples by microbeam X-ray fluorescence spectroscopy was completed. The research included testing the homogeneity of existing standards for X-ray fluorescence calibration and verification of a fundamental parameters method for quantitative analysis. The goal was to evaluate the X-ray fluorescence spectrometer as a tool for elemental analysis at the microscale level. Glass Standard Reference Materials were analyzed. The glass specimens consisted of flat, optically polished slabs having three different thicknesses. For calibration, metal thin films were used. The microbeam X-ray fluorescence spectrometer utilizing capillary optics with effective beam diameter equal to about 30 μm has been applied in this research. Sources of uncertainties considered in this work were detector and X-ray tube stability, specimen movement, and spectral deconvolution. Concentrations of analytes were calculated using a fundamental parameters approach. Coherently and incoherently scattered lines of tube target were used for matrix correction and to estimate the mass thickness of the sample. The synchrotron microbeam X-ray fluorescence technique was used for quantitative analysis of human brain tissue samples. In measurements the monochromatic and polychromatic synchrotron microbeams were applied. The same area of tissue sample was scanned with the use of both X-ray microbeams. The concentrations of selected elements were computed. A reasonably good agreement between results of both analyses was obtained

  6. X-ray fluorescence logging in molybdenum deposit exploration

    Described is the methods for X-ray fluorescence logging in molybdenum deposit exploration in South Kazakhstan. X-ray fluorescence logging was carried out with GKS-1N four-channel gamma spectrometer with SP-4 hole device containing clamping. 109Cd isotope of 10μCi activity was used as a source for excitation of characteristic radiation of molybdenum K-line (E=22 keV, T=470 days) and a proportional counter with the resolution of 12% along 125Sb (E=27 keV) line was used as a detector. Described are methods for interpretation of X-ray flUorescence logs using a nomogram for molybdenum determination in holes filled with water. The sensitivity threshold is 0.05% of molybdenum. Economic efficiency of deposit exploration with the help of holes and subsequent X-ray fluorescence logging is 2.8 mln roubles

  7. X-ray fluorescence analysis of uranium concentrates

    Uranium concentrates were analyzed by x-ray fluorescence for the following impurities: arsenic, calcium, iron, molybdenum, phosphorus, silicon, sulfur, thorium, and vanadium. All of the impurities except arsenic can be determined simultaneously

  8. System for Gamma an X rays fluorescence spectrometric

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  9. Characterization of small particles by micro X-ray fluorescence

    Micro X-ray fluorescence was used to study both homogeneous and heterogeneous particle systems. Specifically, homogeneous glass microspheres and heterogeneous soil particle samples were prepared by both bulk and single particle sample preparation methods for evaluation by micro X-ray fluorescence. Single particle sample preparation methods allow for single particles from a collected sample to be isolated and individually presented to the micro X-ray fluorescence instrument for analysis. Various particle dispersion methods, including immobilization onto Tacky DotTM slides, mounting onto double-sided sticky tape affixed to polypropylene film, or attachment to polypropylene film using 3M Artist's Adhesive, were used to separate the sample particles for single particle analysis. These methods were then compared and evaluated for their ability to disperse the particles into an array of single separated particles for optimal micro X-ray fluorescence characterization with minimal background contribution from the particle mounting surface. Bulk methods of particle sample preparation, which included pellet preparation and aerosol impaction, used a large quantity of collected single particles to make a single homogeneous specimen for presentation to the instrument for analysis. It was found that single particle elemental analysis by micro X-ray fluorescence can be performed if the particles are well separated (minimum separation distance = excitation source beam diameter) down to a particle mass of ∼ 0.04 ng and a mean particle diameter of ∼ 0.06 μm. Homogeneous particulates can be adequately characterized by micro X-ray fluorescence using either bulk or single particle analysis methods, with no loss of analytical information. Heterogeneous samples are much harder to characterize, and both single particle as well as bulk analyses must be performed on the sample to insure full elemental characterization by micro X-ray fluorescence

  10. X-ray fluorescence (XRF) set-up with a low power X-ray tube.

    Gupta, Sheenu; Deep, Kanan; Jain, Lalita; Ansari, M A; Mittal, Vijay Kumar; Mittal, Raj

    2010-10-01

    The X-ray fluorescence set-up with a 100 W X-ray tube comprises a computer controlled system developed for remote operation and monitoring of tube and an adjustable stable 3D arrangement to procure variable excitation energies with low scattered background. The system was tested at different filament currents/anode voltages. The MDL of the set-up at 0.05-1.00 mA/4-12 kV is found approximately (1-100)ppm for K and L excitations and approximately (200-700)ppm for M excitations of elements and improves with filament current and anode voltage. Moreover, L measurements for Sm and Eu at five K X-ray energies of elements(Z=29-40) and analytical determination in some synthetic samples were undertaken. PMID:20570160

  11. X-ray fluorescence (XRF) set-up with a low power X-ray tube

    Gupta, Sheenu; Deep, Kanan [Nuclear Science Laboratories, Physics Department, Punjabi University, Patiala 147 002 (India); Jain, Lalita; Ansari, M.A. [Laser Electronic Support Section, Raja Ramanna Centre for Advanced Technology (RRCAT), Indore (India); Mittal, Vijay Kumar [Nuclear Science Laboratories, Physics Department, Punjabi University, Patiala 147 002 (India); Mittal, Raj, E-mail: rmsingla@yahoo.co [Nuclear Science Laboratories, Physics Department, Punjabi University, Patiala 147 002 (India)

    2010-10-15

    The X-ray fluorescence set-up with a 100 W X-ray tube comprises a computer controlled system developed for remote operation and monitoring of tube and an adjustable stable 3D arrangement to procure variable excitation energies with low scattered background. The system was tested at different filament currents/anode voltages. The MDL of the set-up at 0.05-1.00 mA/4-12 kV is found {approx}(1-100) ppm for K and L excitations and {approx}(200-700) ppm for M excitations of elements and improves with filament current and anode voltage. Moreover, L measurements for Sm and Eu at five K X-ray energies of elements(Z=29-40) and analytical determination in some synthetic samples were undertaken.

  12. Investigation of total reflection X-ray fluorescence analysis technique

    Total-Reflection X-ray Fluorescence spectrometry (TRXF) is known for its high sensitivity down to Pg-level or sub ppb level, respectively. Therefore the spectrometry is considered as a most competitive tool in the application of trace element analysis. The technique of TRXF was investigated in the laboratory. But small isotope X-γ source is chosen as an exciting source instead of general X-ray tube. From the primitive experiment the conclusion proved that the condition of total reflection can be built and the analysis sensitivity of TRXF is higher than that of normal x-ray analysis

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

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

  14. X-ray fluorescence cross sections for K and L x rays of the elements

    Krause, M.O.; Nestor, C.W. Jr.; Sparks, C.J. Jr.; Ricci, E.

    1978-06-01

    X-ray fluorescence cross sections are calculated for the major x rays of the K series 5 less than or equal to Z less than or equal to 101, and the three L series 12 less than or equal to Z less than or equal to 101 in the energy range 1 to 200 keV. This calculation uses Scofield's theoretical partical photoionization cross sections, Krause's evaluation of fluorescence and Coster-Kronig yields, and Scofield's theoretical radiative rates. Values are presented in table and graph format, and an estimate of their accuracy is made. The following x rays are considered: K..cap alpha../sub 1/, K..cap alpha../sub 1/,/sub 2/, K..beta../sub 1/, K..beta../sub 1/,/sub 3/, L..cap alpha../sub 1/, L..cap alpha../sub 1/,/sub 2/, L..beta../sub 1/, L..beta../sub 2/,/sub 15/, L..beta../sub 3/, Ll, L..gamma../sub 1/, L..gamma../sub 4/, and L/sub 1/ ..-->.. L/sub 2/,/sub 3/. For use in x-ray fluorescence analysis, K..cap alpha.. and L..cap alpha.. fluorescence cross sections are presented at specific energies: TiK identical with 4.55 keV, CrK identical with 5.46 keV, CoK identical with 7.00 keV, CuK identical with 8.13 keV, MoK..cap alpha.. identical with 17.44 keV, AgK identical with 22.5 keV, DyK identical with 47.0 keV, and /sup 241/Am identical with 59.54 keV. Supplementary material includes fluorescence and Coster--Kronig yields, fractional radiative rates, fractional fluorescence yields, total L-shell fluorescence cross sections, fluorescence and Coster-Kronig yields in condensed matter, effective fluorescence yields, average L-shell fluorescence yield, L-subshell photoionization cross section ratios, and conversion factors from barns per atom to square centimeters per gram.

  15. X-ray fluorescence in IAEA Member States: Peru

    Full text: Under the IAEA TC project PER/2/018 (1993-1994) on 'Nuclear Training' an EDXRF spectrometer based on Cd-109 radioisotope source was installed. Then in 1998 a Total Reflection X-ray Fluorescence module was attached under the project PER/9/020 on 'Analytical Nuclear Techniques for Environmental Control'. The XRF laboratory belongs to the Chemistry Department of Science Direction - General Direction for Promotion and Technical Development of the Peruvian Institute of Nuclear Energy and is located at the auxiliary laboratories of the Nuclear Centre. The following three thesis for degree in chemistry were completed: 1. 'Multielemental Analysis of archeological bones by X-ray Fluorescence for the reconstruction of diets at First Period in the Lima Culture'; 2. 'Determination of heavy metals in water of the Rimac river by Total Reflection X-Ray Fluorescence'; 3. 'Multielemental Analysis of sea water samples by Total Reflection X-Ray Fluorescence, using pre-concentration with APDC/MIBK' (in edition). Currently we are working on another thesis dealing with 'Multielemental analysis of biological marine samples by Total Reflection X-Ray Fluorescence and pre-concentration after microwave digestion'. In order to get the accreditation, we are working on validation of the analytical methods for determination of Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se and Pb in natural water by using Total Reflection X-Ray Fluorescence technique. The EDXRF spectrometer with Cd-109 excitation is used for the analysis of clays, potteries, soil, sediments, geological materials, bones, etc., mainly for the archaeological applications. (author)

  16. X-ray fluorescence microtomography analyzing prostate tissues

    The objective of this work is to determine the elemental distribution map in reference samples and prostate tissue samples using X-Ray Fluorescence Microtomography (XRFCT) in order to verify concentrations of certain elements correlated with characteristics observed by the transmission microtomography. The experiments were performed at the X-Ray Fluorescence Facility of the Brazilian Synchrotron Light Laboratory. A quasi-monochromatic beam produced by a multilayer monochromator was used as an incident beam. The transmission CT images were reconstructed using filtered-back-projection algorithm, and the XRFCT images were reconstructed using filtered-back-projection algorithm with absorption corrections. (author)

  17. Research status of energy dispersive X-ray fluorescence spectrometer

    Background: Energy dispersive X-ray fluorescence spectrometer has been improved rapidly in these years. Purpose: Research status of energy dispersive X-ray fluorescence spectrometers is reviewed, covering the main components in the spectrometer and spectra processing algorithms. Methods: On the component aspect, the working principles and performances of high-voltage generator, X-ray excitation sources, especially X-ray tubes and detector are compared. On the spectra processing aspect, results of different algorithms in spectrum de-noising, background subtraction, decomposition of the peaks and calculating the intensity of the fluorescence are analyzed separately. Results: On the component aspect, the effects to sensitivity and resolution of the spectrometer being caused by the high-voltage of the voltage generator, intensity of X-ray and resolution of the detector are concluded. On the spectra processing aspect, feasibilities of various algorithms are suggested. The advantages of wavelet transform, artificial neural network and partial least-squares method are discussed. Conclusion: Present difficulties in further improving of the spectrometer performance are analyzed. The prospect and the necessity of further research of EDXRF have been suggested. (authors)

  18. X-ray-fluorescence measurement of thin film thicknesses

    A method and apparatus were developed for X-ray fluorescence measurement of the thicknesses of thin metal films deposited on top of each other on a substrate. The method is highly accurate and rapid and is especially useful for making microelectronic devices. The system involves exposing the metal films to X-ray radiation, then measuring the intensity of the various fluorescent lines excited by the radiation. The lead-detecting collimator has a conical bore and a very small entrance aperture used to define the surface area of the top film from which excited fluorescence is to be detected. The collimator has an opening in the side to allow some of the incident X-rays from the source to enter the bore to excite fluorescence in the lead. This fluorescence is monitored by a detector as a measure of the intensity of the incident X-rays. The system is first calibrated in a systematic way to specify a set of parameters characteristic of the plated-metal configuration to be measured. The sample is irradiated and the number of counts in each of the selector characteristic lines of the platings and substrate is measured. The thickness of the plating layers are then calculated by an iterative method in accordance with specified relationships between the calibrated parameters and the measured counts. (DN)

  19. X-ray fluorescence analysis major elements in silicate minerals

    Hagan, R.C.

    1982-09-01

    An automated wavelength-dispersive x-ray fluorescence spectrometer is operational for analysis of major elements in rocks and minerals. Procedures for trace-element analysis are being developed. Sample preparation methods and analytical techniques are similar to those commonly used elsewhere, but data reduction is conducted by the Fundamental Parameters program developed by Criss. Unlike empirically derived calibration curves, this data reduction method considers x-ray absorption and secondary fluorescence, which vary with differences in sample composition. X-ray intensities for each element from several standards are averaged to develop a theoretical standard for comparison with samples of unknown composition. Accurate data for samples with wide compositional ranges result from these data reduction and standardization techniques.

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

    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.

  1. Quantitative X ray analysis system. User's manual and guide to X ray fluorescence technique

    This guide covers trimmed and re-arranged version 3.6 of the Quantitative X ray Analysis System (QXAS) software package that includes the most frequently used methods of quantitative analysis. QXAS is a comprehensive quantitative analysis package that has been developed by the IAEA through research and technical contracts. Additional development has also been carried out in the IAEA Laboratories in Seibersdorf where QXAS was extensively tested. New in this version of the manual are the descriptions of the Voigt-profile peak fitting, the backscatter fundamental parameters' and emission-transmission methods of chemical composition analysis, an expanded chapter on the X ray fluorescence physics, and completely revised and increased number of practical examples of utilization of the QXAS software package. The analytical data accompanying this manual were collected in the IAEA Seibersdorf Laboratories in the years 2006/2007

  2. HIgh Rate X-ray Fluorescence Detector

    Grudberg, Peter Matthew [XIA LLC

    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

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

    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.

  4. USB apply to field X-ray fluorescence analysis

    This article analyzes the feasibility of application USB and GPS to field X-ray fluorescence analysis, and focuses on the hardware and firmware design of USB and multi-channel analyzer (MCA), then simply discusses the device driver design and the PC application software design. (authors)

  5. Characterization of monel alloys by X-ray fluorescence technique

    Method for the determination of Ni, Cu, Fe, Mn, Si, Al, Ti, Co, Cr and Mo in Monel alloys using thin film for sample preparation and X-ray fluorescence techniques is described. Samples in filings form were completely dissolved with inorganic acids and they were made up to a known volume. Then, these samples were deposited in a filter paper, reducing in this form the effect of the matrix. For all elements the first order emission Kα lines were selected for measurements and for excitation a rhodium X-ray tub was utilized. For the heavier elements the LiF (200). (author)

  6. Rapid analysis by X-ray fluorescence excitation

    The application of the energy dispersive X-ray fluorescence spectrometry for a quick multielement analysis of different samples (sedimented dust, motor oil, watery solutions) is discussed. Using a source of 30 mCi 239Pu for the X-ray excitation it is possible to determine the concentration of the elements Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Br, Sr, and Pb in a single working operation with a detection efficiency between 1000 ppm for Ca and about 10 ppm for Zn, Br, Sr and Pb using a testing time of 1000 seconds. (author)

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

    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%. PMID:24004868

  8. Effect of Electric Voltage and Current of X-ray Chamber on the Element inthe Zirconium Alloy Analysis X-ray by X-ray Fluorescence

    The using of x-ray fluorescence in the chemical analysis depend heavilyon the parameters of x-ray chamber, for examples : electric voltage andelectric current. That parameter give effect in the result of determine ofSn, Cr, Fe and Ni in the zirconium alloy. 20 kV electric voltages are used onthe Mo x-ray chamber shall product x-ray of zirconium in the sample materialcan give effect in the stability of the analysis result (deviation more than5%). The result of analysis of elements in the zirconium alloy shall givedeviation less than 5% when using of electric voltage of the x-ray chamberless than 19 kV. The sensitivity of analysis can be reached by step upelectric current of x-ray chamber. (author)

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

    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.

  10. Proton-induced x-ray fluorescence CT imaging

    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

  11. Proton-induced x-ray fluorescence CT imaging

    Bazalova-Carter, Magdalena, E-mail: bazalova@stanford.edu; Xing, Lei [Department of Radiation Oncology, Stanford University, Stanford, California 94305-5847 and Global Station for Quantum Medical Science and Engineering, Global Institution for Collaborative Research and Education (GI-CoRE), Hokkaido University, Sapporo 060-8648 (Japan); Ahmad, Moiz [Department of Radiation Oncology, Stanford University, Stanford, California 94305-5847 (United States); Matsuura, Taeko; Takao, Seishin; Shirato, Hiroki; Umegaki, Kikuo [Department of Medical Physics, Proton Beam Therapy Center, Hokkaido University Hospital, Sapporo 060-8648, Japan and Global Station for Quantum Medical Science and Engineering, Global Institution for Collaborative Research and Education (GI-CoRE), Hokkaido University, Sapporo 060-8648 (Japan); Matsuo, Yuto [Department of Medical Physics, Proton Beam Therapy Center, Hokkaido University Hospital, Sapporo 060-8648 (Japan); Fahrig, Rebecca [Department of Radiology, Stanford University, Stanford, California 94305 (United States)

    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

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

    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

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

    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.

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

    Emoto, T.; Sato, Y.; Konishi, Y.; Ding, X.; Tsuji, K. E-mail: tsuji@a-chem.eng.osaka-cu.ac.jp

    2004-08-31

    A polycapillary X-ray lens is an effective optics to obtain a {mu}m-size X-ray beam for micro-X-ray fluorescence spectrometry ({mu}-XRF). We developed a {mu}-XRF instrument using a polycapillary X-ray lens, which also enabled us to perform Grazing Exit {mu}-XRF (GE-{mu}-XRF). The evaluated diameter of the primary X-ray beam was 48 {mu}m 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-{mu}-XRF. We expect that GE-{mu}-XRF will become an effective method of estimating the film thickness of a small region.

  15. Total Reflection X Ray Fluorescence: an approach to nano analysis

    Within the last decade, Total Reflection X Ray Fluorescence (TXRF) has become an extremely powerful method of element analysis. It allows nanoanalytical investigations in three different ways: (i) use of minute sample amounts of only some 100 nanograms, (i i) determination of extreme traces down to nanograms per liter and (i i i) depth profiling of near surface layers of only 10 nanometer thickness. The basic principles of TXRF are described and examples of applications are demonstrated

  16. Survey of realization possibilities in X-ray fluorescence analysis

    X-ray fluorescence analysis is reviewed as a method of quantitative chemical analysis. Physical basis of the method and the sample preparation process, having an important effect on the sensitivity and accuracy of the method, are briefly described. Different realization and equipment construction possibilities are discussed in detail, including the method of non-dispersive or differential filter pair which leads to the decrease of measuring time and statistical errors. (D.Gy)

  17. Analysis of silicate rocks by x-ray fluorescence spectrometry

    This study aims at developing an all-purpose method for the determination of various elements in silicate rocks, by means of X-ray fluorescence spectrometry. The sample is prepared by borax fusion, in the presence of cobalt oxide acting as an inner standard meant for eliminating certain errors. Contents are computed in comparison with outer standards having a chemical composition akin to that of the rock sample under analysis. (authors)

  18. In vivo X-ray fluorescence analysis for medical diagnosis

    A Monte Carlo code has been constructed and used to simulate the energy distribution of scattered photons abtained in various in vivo X-ray fluorescence measurements. The structure of this distribution has been investigated and discussed. Studies of the response function of the Ge-decector used have made it possible to convert the calculated scatter spectra to pulse-height distributions. These studies have shown to be valuabel tools in designing in vivo X-ray fluorescence measurements. In vivo X-ray fluorescence measurements have been used for quantitative non-invasive measurements of the concentration of iodine-containing contrast media in rabbits without the use of blood or urine sampling. The biological half-life of the contrast medium in the soft tissue part of the nose (measured in vivo) was similar to that in serum (measured in vitro) when determined in the period 2-4 hours after injection. This result indicate the possibility of being able to use the method for clinical evaluation of kidney function. The method has been used in patients referred for urography and who had teherefore been injected with routine amounts of iodinecontaining urographic contrast medium. After urography, the elimination rates of urographic contrast medium from both serum and finger tissue were determined and copared during a two-hour period which began two hours after injection of contrast medium. A strong degree of correlation was found between the elimination rates from serum and finger tissue and also between the total clearances calculated from the serum and finger measurements respectively. Thus, after radiographic examinations quantitative estimation of kidney function may be obtained as a fringe benefit by external X-ray fluorescence measurements of the elimination from tissue of the contrast medium used. (author)

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

    Groover, Krishangi; Izbicki, John

    2016-01-01

    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.

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

    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. ...

  1. Portable x-ray fluorescence spectrometer for Works of art

    X-ray fluorescence is an analytical technique of prier importance in archaeometry, for restoration and art history investigation; it is because of non-destructive and multi-elemental character of the analysis simplicity and high speed of operation, ability to produce immediate analytical results for the objects, which can neither be sampled nor removed to the laboratory Recent advances in X-ray tubes, X-ray detectors and electronic provided an opportunity to produce portable high resolution XRF spectrometers characterized by a good reliability and analytical performance; in this paper a prototype portable XRF spectrometer based on a small size, low power X-ray tube and a thermometrically cooled Si-Pin detector is described. The spectrometer provides a possibility for direct and secondary target excitation geometry use of proper secondary target and filter and size adjustment of the primary photon bean by using a set of different beam collimators; the portable XRF spectrometer was successfully applied to study art objects in the Art History Museum in Vienna, including such objects as old master paintings bronze and brass alloys of antique as well as Renaissance objects and silver/copper coins produced at different locations. Quantitative and Quantitative analysis were amedee depending of the curator questions and discussed from the point of view of art History. The importance of the results for restoration and authentification of the art objects is also emphasized

  2. Applications of synchrotron x-ray fluorescence to extraterrestrial materials

    Sutton, S.R.; Rivers, M.L.; Smith, J.V.

    1986-01-01

    Synchrotron x-ray fluorescence (SXRF) is a valuable technique for trace element analyses of extraterrestrial materials permitting minimum detection limits less than 1 ppM for 20 micrometer spots. SXRF measurements have been performed on iron meteorites and micrometeorites using white synchrotron radiation and an energy dispersive x-ray detector at the National Synchrotron Light Source (X-26C), Brookhaven National Laboratory (NY). Partitioning of Cu between troilite (FeS) and metal in the nine iron meteorites studied suggests sub-solidus re-equilibration in these objects. A technique has been developed for determining self-absorption corrections for filtered, continuum excitation of small specimens, such as stratospheric particles and refractory inclusions in meteorites.

  3. Hybrid fluorescence tomography/x-ray tomography improves reconstruction quality

    Schulz, R. B.; Ale, A.; Sarantopoulos, A.; Freyer, M.; Söhngen, R.; Zientkowska, M.; Ntziachristos, V.

    2009-07-01

    A novel hybrid imaging system for simultaneous X-ray and Fluorescence Tomography is presented, capitalizing on 360°-projection free-space fluorescence tomography. The system is implemented within a commercial micro-CT scanner allowing reconstructions with a resolution of 95μm. Acquired data sets are intrinsically coregistered in the same coordinate system and can be used to correctly localize reconstructed fluorescence distributions with morphological features. More importantly, the micro-CT data, automatically segmented into different organ and tissue segments can be used to guide the fluorescence reconstruction algorithm and reduce the ill coditioning of the inverse problem. We showcase the use of the system and the improvements in image quality for lesions in brain and lung.

  4. X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation - Modelling, experiment, and Monte-Carlo simulation

    Hodoroaba, V.-D., E-mail: Dan.Hodoroaba@bam.d [BAM Federal Institute for Materials Research and Testing, Division VI.4 Surface Technologies, D-12200 Berlin (Germany); Radtke, M. [BAM Federal Institute for Materials Research and Testing, Division I.3 Structure Analysis, Polymer Analysis, D-12200 Berlin (Germany); Vincze, L. [Ghent University, Department of Analytical Chemistry, B-9000 Ghent (Belgium); Rackwitz, V.; Reuter, D. [BAM Federal Institute for Materials Research and Testing, Division VI.4 Surface Technologies, D-12200 Berlin (Germany)

    2010-12-15

    X-ray scattering may contribute significantly to the spectral background of X-ray fluorescence (XRF) spectra. Based on metrological measurements carried out with a scanning electron microscope (SEM) having attached a well characterised X-ray source (polychromatic X-ray tube) and a calibrated energy dispersive X-ray spectrometer (EDS) the accuracy of a physical model for X-ray scattering is systematically evaluated for representative samples. The knowledge of the X-ray spectrometer efficiency, but also of the spectrometer response functions makes it possible to define a physical spectral background of XRF spectra. Background subtraction relying on purely mathematical procedures is state-of-the-art. The results produced by the analytical model are at least as reliable as those obtained by Monte-Carlo simulations, even without considering the very challenging contribution of multiple scattering. Special attention has been paid to Compton broadening. Relevant applications of the implementation of the analytical model presented in this paper are the prediction of the limits of detection for particular cases or the determination of the transmission of X-ray polycapillary lenses.

  5. X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation - Modelling, experiment, and Monte-Carlo simulation

    X-ray scattering may contribute significantly to the spectral background of X-ray fluorescence (XRF) spectra. Based on metrological measurements carried out with a scanning electron microscope (SEM) having attached a well characterised X-ray source (polychromatic X-ray tube) and a calibrated energy dispersive X-ray spectrometer (EDS) the accuracy of a physical model for X-ray scattering is systematically evaluated for representative samples. The knowledge of the X-ray spectrometer efficiency, but also of the spectrometer response functions makes it possible to define a physical spectral background of XRF spectra. Background subtraction relying on purely mathematical procedures is state-of-the-art. The results produced by the analytical model are at least as reliable as those obtained by Monte-Carlo simulations, even without considering the very challenging contribution of multiple scattering. Special attention has been paid to Compton broadening. Relevant applications of the implementation of the analytical model presented in this paper are the prediction of the limits of detection for particular cases or the determination of the transmission of X-ray polycapillary lenses.

  6. Analysis of fresco paintings by X-ray fluorescence method

    In this work we present the application of X-ray fluorescence analysis (XRFA) to examine fresco paintings from the Karlstejn castle. The X-ray fluorescence apparatus built and operated in the Laboratory of Quantitative Methods in Research of Ancient Monuments was used for the purpose of fresco paintings measurements. The X-ray sources (radionuclides) generate the characteristic X-ray photons from the sample. The Si(Li) detector measures numbers and energies of photons emitted from the specimen. The energy and number of photons detected can be converted into kind and amount of measured atoms. These results give data for qualitative and quantitative analysis of samples. XRFA is relatively simple and non-destructive method. Capability of in-situ measurement is one of big advantages of this method. The radionuclide sources of exciting radiation (e.g. 55Fe enables the excitation of elements with Z up to 23, 238Pu is used in interval of Z from 20 to 39 etc.) were used. An Si(Li) semiconductor detector with a 5 l Dewar vessel and portable spectroscopy system enable the in situ measurement. Narrow collimation of the exciting beam makes it possible to select the measured area of fresco painting. The valuable fresco paintings from the Karlstejn castle were investigated in this way. The measurements were carried out in collaboration with the Analytical Laboratory of the State Institute for the Preservation of Historic Monuments. A suitable analysis of paintings makes it possible to detect the kind of colours and evaluate changes in the surface colour of paintings and suggest useful and timely procedures for their conservation and restoration. (author)

  7. X-ray fluorescence in IAEA Member States: Spain

    Full text: Instrumental facilities of the ICMUV include: a Total-reflection X-Ray Fluorescence (TXRF), laboratory and portable Energy Dispersive X-Ray Fluorescence (EDXRF) spectrometers. These equipments are employed in the field of the art and archaeometry. Current projects are: EDXRF analysis of blue pigments used in Valencian ceramics. EDXRF analyses of cobalt-blue pigments were made on 73 pieces of Valencian ceramics from the beginning of the 14th century up to 20th century. These ceramic samples have the pigment decoration applied together with a tin opacified lead glaze cover on the clay body. The comparison between EDXRF spectra from coloured and non-coloured areas provides information about the pigment composition. The following elements: Mn, Fe, Co, Ni, Cu, Zn and As are identified as characteristics of the blue pigments. Different association of these elements as well as correlation with the chronology of the samples were found. These results can be used for identifying the different types of cobalt ores employed in the manufacture of the blue pigments to study their provenance. Non-destructive analysis of paper supports used in prints: In paper based works of art it is not possible to separate the support from the work of the author. Then, the maximum knowledge of the support in this kind of works is desirable. In this work, Energy Dispersive X-Ray Fluorescence (EDXRF) was used to determine the elemental composition of a set of European and Oriental papers from the 20th century and an Arabian paper from the 14th century. These papers were manufactured with different production techniques and used as support for writing, drawing and printing. Normalised fluorescence yields of the elements to the weight of the paper show that there are some correlations between its elemental composition and the type of paper, provenance and use. Therefore, the Energy Dispersive X-Ray Fluorescence (EDXRF) technique could be used for a better characterization and

  8. X-ray fluorescence in Member States: Slovenia. Applications of X ray fluorescence spectrometry in biology and food science

    Our objective here is to present briefly two applications of the XRF elemental analysis, which we recently started: applying the XRF analysis after sample excitation by radioisotope sources, X ray tubes in the standard and the total reflection modes (TXRF), as well as by PIXE and microPIXE. The fluorescence X ray spectra shown below are typical examples of data and information on basis of which all the applications were realized. It is obvious that the use of the techniques, which produce the above spectra require a good knowledge of the nuclear spectroscopy, and also skills to adjust the experimental set-up including the source of fluorescence excitation, selection of appropriate X ray detection system (geometry of experiment), as well as proper sampling and sample preparation, considering the characteristics of a large variety of different materials to be examined. And finally one needs to define the application and establish good collaboration with the users and/or scientists in a number of interesting fields. We would like to present here just two examples of such a comprehensive approach to the application of XRF analysis

  9. X-ray Peltier cooled detectors for X-ray fluorescence analysis

    The recent results on development of X-ray Si(Li), Si-planar and CdTe p-i- n detectors cooled by Peltier coolers for fabrication of laboratory and portable XRF analysers for different applications are discussed. Low detection limits of XRF analysers are provided by increasing of detectors sensitive surface; improvement of their spectrometrical characteristics; decreasing of front-end-electronics noise level; Peltier coolers and vacuum chambers cooling modes optimization. Solution of all mentioned tasks allowed to develop Peltier cooled detectors with the following performances: (1) Si(Li) detectors: S = 20 mm2, thickness = 3.5 mm, 175 eV (5.9 keV), 430 eV (59.6 keV); S = 100 mm2; thickness = 4.5 mm, 270 eV (5.9 keV), 485 eV (59,6 keV). (2) Si-planar detector: S = 10 mm2, thickness = 0.4 mm, 230 eV (5.9 keV), 460 eV (59.6 keV). (3) CdTe p-i-n detectors: S = 16 mm2, thickness 0.5 mm, 350 eV (5.9 keV), 585 eV (59.6 keV). S = 16 mm2, thickness = 1.2 mm, 310 eV (5.9 keV), 600 eV (59.6 keV). Advantages and disadvantages of all types of detectors for X-ray fluorescence analysis are compared. Spectra are presented. Application of different XRF analysers based on developed detectors in medicine, environmental science, industry, criminalistics and history of art are demonstrated. (author)

  10. Rare earth aerosol analysis by x-ray fluorescence spectrometry

    An analytical method for the determination of four lanthanides in air filter samples is described. The method involves simultaneous quantitative determinations of La, Ce, Pr, and Nd at the microgram level by x-ray fluorescence spectrometry without chemical separation of these rare earths and without serious interferences from the dust matrices on the filters. The method has been used successfully to analyze some air filter samples collected at a rare earth processing refinery in Illinois. A description of the development of the method is given as well as the results obtained by using this method on the air filter samples. The reproducibility of the results was generally +-5%

  11. X-ray fluorescence analysis of welding fume particles

    A commercial standard filter set and two laboratory-made standard filter sets are compared via the analysis of generated welding fume samples by X-ray fluorescence. The latter standards are made by (1) hydrophobic-edge membrane filters spiked with prepared metal ion solutions, and (2) filters through which a dispersion of metal oxide powder in isopropanol has been drawn. The results are presented in table form. Precision (Pre) is the relative standard deviation of the six samples. Four main conclusions are enumerated

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

    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.

  13. Analysis of archaeological ceramics using x-ray fluorescence technique

    Radioisotope x-ray fluorescence method was applied to provenance studies of ceramics fragments originated from the Mar-Takla site in Syria. 35 samples were analyzed, where each sample was irradiated 1000 s by 109Cd radioisotope source and the elements (As, Ca, fe, Ga, Nb, Mn, Pb, Rb, Sr, Ti, Y, Zn, and Zr) were determined. The data were subjected to two multivariate statistical methods, cluster and principal component analysis (PCA). The study show that 94% of the samples can be considered to be manufactured using two sources of raw materials. (Author)

  14. Analysis of industrial material with X ray fluorescence

    The content of selenium in a calcium carbonate based fodder additive was determined by X ray fluorescence (XRF) analysis using radionuclide excitation. The aim was to develop a fast and uncomplicated technique that could be used on-site, for example in a factory or in other places of industrial scale production of material. The selenium contents to be determined were around 4-5 mass per cent in the additive, which is produced in tonne quantities; hence emphasis was placed upon the mobility and simplicity of the device rather than upon the possibility of analysis of small traces

  15. Blood selenium content determination by X-ray fluorescence

    The presence of some elements in small amounts (traces) in the human body is of foremost importance for the prevention and treatment of several diseases. It has been recently shown that traces of selenium in blood are closely related to the occurrence of miotonic distrophy, a muscular disease that is affecting a significant percentage of the population. This work describes a simple procedure to determine selenium in human blood serum by energy dispersive X-ray fluorescence analysis. Final quantification is achieved through the addition of titanium as an internal standard. (Author)

  16. Studies of some alloys using x-ray fluorescence

    In this project an attempt has been made for the study of alloys commonly used using x-ray fluorescence ( XRF ) technique. The alloys selected for the study included gold jewellery, steels, brasses and coins. The XRF method proved to be simple, fast, non-destructive and reliable as compared to chemical methods. The results showed that most of the gold jewellery used in this country have carat value of 18 and 21. Also most coins used in different countries are alloys of Cu and Ni. A simple spark method was used for the determination of C in steels, since C is not possible to analyze by XRF. ( Author )

  17. X-Ray Diffraction and X-Ray Fluorescent Analyses of Prehistoric Pottery Shards from Ulu Kelantan

    Zuliskandar Ramli; Nik H.S.N. Abdul Rahman; Adnan Jusoh; Yunus Sauman

    2011-01-01

    Problem statement: X-Ray Diffraction (XRD) and X-Ray Fluorescent (XRF) were used in order to obtain mineralogical and elemental composition of seven pottery shards that have been unearthed during the excavation at Peraling Cave and Cha Cave in Ulu Kelantan, Malaysia. Approach: Peraling Cave and Cha Cave were prehistoric sites dating from 10, 000 BC which were inhabited by Hoabinhian people and then continuously used by people of Neolithic culture around 3000 BC. Results: Mineralogical and ele...

  18. X-ray scattering in X-ray fluorescence spectra with X-ray monochromatic, polarised excitation - Modelling, experiment, and Monte-Carlo simulation

    Hodoroaba, V.-D., E-mail: Dan.Hodoroaba@bam.de [BAM Federal Institute for Materials Research and Testing, Division 6.4 Surface Technologies, D-12200 Berlin (Germany); Radtke, M.; Reinholz, U.; Riesemeier, H. [BAM Federal Institute for Materials Research and Testing, Division 1.3 Structure Analysis, Polymer Analysis, D-12200 Berlin (Germany); Vincze, L. [Ghent University, Department of Analytical Chemistry, B-9000 Ghent (Belgium); Reuter, D. [BAM Federal Institute for Materials Research and Testing, Division 6.4 Surface Technologies, D-12200 Berlin (Germany)

    2011-07-01

    A systematic series of measurements has been carried out with monochromatic X-ray excitation with synchrotron radiation in order to check a physical model on X-ray scattering. The model has recently been successfully tested for the case of polychromatic, unpolarised excitation emitted by an X-ray tube. Our main purpose is the modelling of a physical background in X-ray fluorescence spectra, so that improved quantitative results can be achieved especially for strongly scattering specimens. The model includes single Rayleigh and Compton scattering in the specimen, the effect of bound electrons, the challenging Compton broadening and the polarisation degree. Representative specimens, measurement geometries and excitation energies have been selected with synchrotron monochromatic light at BAMline/BESSY II. Monte-Carlo simulations have been also carried out in order to evaluate the quality of the results achieved with the model.

  19. X-ray scattering in X-ray fluorescence spectra with X-ray monochromatic, polarised excitation - Modelling, experiment, and Monte-Carlo simulation

    A systematic series of measurements has been carried out with monochromatic X-ray excitation with synchrotron radiation in order to check a physical model on X-ray scattering. The model has recently been successfully tested for the case of polychromatic, unpolarised excitation emitted by an X-ray tube. Our main purpose is the modelling of a physical background in X-ray fluorescence spectra, so that improved quantitative results can be achieved especially for strongly scattering specimens. The model includes single Rayleigh and Compton scattering in the specimen, the effect of bound electrons, the challenging Compton broadening and the polarisation degree. Representative specimens, measurement geometries and excitation energies have been selected with synchrotron monochromatic light at BAMline/BESSY II. Monte-Carlo simulations have been also carried out in order to evaluate the quality of the results achieved with the model.

  20. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface Project

    National Aeronautics and Space Administration — We propose to develop a compact and lightweight X-Ray Diffraction (XRD) / X-Ray Fluorescence (XRF) instrument for analysis of mineralogical composition of regolith,...

  1. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface Project

    National Aeronautics and Space Administration — We propose to develop LUNA, a compact and lightweight X-Ray Diffraction (XRD) / X-Ray Fluorescence (XRF) instrument for mineralogical analysis of regolith, rock...

  2. X-ray fluorescence in Member States: Venezuela

    The direct analysis of biological samples is the main research challenge of the scientific group at the Unidad de Analisis Instrumental of the Agronomy Faculty, Universidad Centro Occidental Lisandro Alvarado, (UCLA) Edo. Lara, Venezuela. The technique of total reflection X-ray fluorescence (TXRF) plays an important role in the scientific activities of the laboratory. In this field, the research is devoted to the design, development, evaluation and application of methods for the analysis of biological and related samples, such as biological tissues, fluids, biota, soil and water samples. The studies involve the evaluation of feasibility for direct determination of analytes, the in situ (in quartz sample holder) preparation techniques, the in situ pre-concentration and speciation among others studies. The methods are developed for the application in clinical studies, agronomy, environmental monitoring, bioremediation, statistical processing of data and neural network applications. The following projects are described: Direct analysis of biological samples by TXRF; Determination of calcium, potassium, manganese, iron, cooper and zinc levels in representative samples of two onion cultivars using TXRF and ultrasound extraction procedure; Evaluation of vermicompost as bioadsorbent substrate of Pb, Ni, V and Cr for waste waters remediation using total reflection X-ray fluorescence; Determination by TXRF of total As in onion plants growing in contaminated substrates

  3. Preparation of tissue samples for X-ray fluorescence microscopy

    Chwiej, Joanna; Szczerbowska-Boruchowska, Magdalena; Lankosz, Marek; Wojcik, Slawomir; Falkenberg, Gerald; Stegowski, Zdzislaw; Setkowicz, Zuzanna

    2005-12-01

    As is well-known, trace elements, especially metals, play an important role in the pathogenesis of many disorders. The topographic and quantitative elemental analysis of pathologically changed tissues may shed some new light on processes leading to the degeneration of cells in the case of selected diseases. An ideal and powerful tool for such purpose is the Synchrotron Microbeam X-ray Fluorescence technique. It enables the carrying out of investigations of the elemental composition of tissues even at the single cell level. The tissue samples for histopathological investigations are routinely fixed and embedded in paraffin. The authors try to verify the usefulness of such prepared tissue sections for elemental analysis with the use of X-ray fluorescence microscopy. Studies were performed on rat brain samples. Changes in elemental composition caused by fixation in formalin or paraformaldehyde and embedding in paraffin were examined. Measurements were carried out at the bending magnet beamline L of the Hamburger Synchrotronstrahlungslabor HASYLAB in Hamburg. The decrease in mass per unit area of K, Br and the increase in P, S, Fe, Cu and Zn in the tissue were observed as a result of the fixation. For the samples embedded in paraffin, a lower level of most elements was observed. Additionally, for these samples, changes in the composition of some elements were not uniform for different analyzed areas of rat brain.

  4. Plating thickness measurement using x-ray fluorescence

    Recently, there has been increased demand for the accurate thickness measurement of the plating on small electronic parts. This technology is required for both production and quality control. The coating thickness measurement using X-ray fluorescence is the standard method used because of its accuracy and versatility. Beta-ray backscattering method is also described. The operation of a beta-ray gauge is fairly simple, and the normal measuring time with it is much shorter than that of other methods. It is one of nondestructive methods, and excellent in view of its accuracy, ease of operation and speed. The engineers of Seiko Instruments and Electronics Ltd. have endeavored to eliminate the weak points of beta-ray backscattering while keeping the instrument as inexpensive as possible. The detection system of X-ray fluorescence (XRF) was complicated and expensive, but the recent development of low cost and compact electronic devices brought the cost of XRF instruments down, thus the widely spread use of XRF advances. The data shows the many advantages of XRF over beta-ray backscattering. The on-line XRF coating thickness gauges for reel to reel plating application are at the forefront of this technology. The use of solid state detectors for XRF gauges to expand the application and to increase energy resolution is a possibility. Any strong competition does not seem to develop against XRF. (Kako, I.)

  5. Applications of EGS4 Monte Carlo simulation for x-ray source characterization and potable x-ray fluorescence spectroscopy

    We applied EGS4 Monte Carlo (MC) simulation to the spectral evaluation of the primary x-ray beam from low-power x-ray tube and the prediction of the energy-dispersive x-ray fluorescence (ED-XRF) analysis of metals. The end-window type of small x-ray tube with Mo anode was adopted to observe the backscattered component of the primary x-ray beam under the condition of low power (<50 kV, <1 μA). For estimation of the filtration effect on the primary x-ray beam, the set of Si and Mo sheet optimized for harmful heavy elements analysis were used. On the other hand, the ED-XRF spectra of metals were recorded using a portable spectrometer with LiF bend monochromator which enables simple measurement situation. In all measurement situations MC calculations were done using low energy extension of EGS4 code, and the experimental data can be compared directly with the simulated spectrum. Results showed that the EGS4 MC calculations are useful method for spectral evaluation of x-ray tube and analysis of ED-XRF measurement. (author)

  6. A low power x-ray tube for use in energy dispersive x-ray fluorescence analysis

    A low power X-ray tube with thin molybdenum transmission target for use in energy dispersive X-ray fluorescence (ENDXRF) element analysis has been indigenously built, along with its power supply. The X-ray tube has been in operation since August 1979, and it has been operated upto maximum target voltage of 35 KV and tube current upto 200 μA which is more than sufficient for trace element analysis. This X-ray tube has been used alongwith the indigenously built Si(Li) detector X-ray spectrometer with an energy resolution of 200 eV at 5.9 Kev MnKsub(α) X-ray peak for ENDXRF analysis. A simple procedure of calibration has been developed for thin samples based on the cellulose diluted, thin multielement standard pellets. Analytical sensitivities of the order of a few p.p.m. have been obtained with the experimental setup for elements with 20 < = Z < = 38 and 60 < = Z < = 90. A number of X-ray spectra for samples of environmental, biological, agricultural, industrial and metallurgical interest are presented to demonstrate the salient features of the experimental sep up. (auth.)

  7. X-ray fluorescence in Member States: United Arab Emirates. United Arab Emirates' National X ray Fluorescence Laboratory

    The United Arab Emirates (UAE) is currently experiencing an era of accelerated development and expansion in all aspects of civil activities. Huge industrial, as well as, construction projects, evident to the casual observer, have resulted in the creation of environmental conditions that need continuous monitoring. In addition to that, wide interest in the heritage and archaeological findings in the UAE, have necessitated the establishment of a national scientific laboratory capable of analyzing a variety of samples non-destructively, with high accuracy and a minimum amount of sample preparation. X ray fluorescence (XRF) is one of a number of methods that are suitable for the type of analysis required. XRF is widely used for chemical analysis, particularly in the investigation of metals, glass, ceramics and building materials, and for applications in environmental sciences, geochemistry, forensic science and archaeology. Moreover, XRF has the advantage of low cost of instrumentation and maintenance over similar techniques. As a result, the UAE, in cooperation with IAEA, is establishing a national X ray fluorescence laboratory (NXFL), hosted by the University of Sharjah, for environmental and cultural heritage applications. The 3 years project was approved by the IAEA under Technical Cooperation Program (Project UAE 0006). Scientists from two institutions, University of Sharjah (UoS) and American University of Sharjah (AUS), will be involved in establishing the lab, training the staff, running outreach workshops within the country and supervising the operation of the laboratory. The core of the scientific team is composed of four professors with excellent knowledge of the subject and extensive experience in utilizing X ray techniques in material science

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

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

  9. X-ray fluorescence in IAEA Member States: Spain

    Full text: The Archaeometry Unit (UA) of the Material Science Institute of the Valencia University (ICMUV) has got portable EDXRF spectrometers with small X-Ray tubes and thermoelectrically cooled semiconductor detectors (Cd(Zn)Te and Si-PIN). In June 2002 a new facility based on Total Reflection X-Ray Fluorescence (TXRF) analysis will also be in operation at the UA. The research activities of the UA include in situ EDXRF analysis of art objects from the Spanish Cultural Heritage. The following examples are worth mentioning: - Identification of the underglaze and overglaze cobalt blue decoration of painted ceramics from Valencia (XIV-XIX centuries). This project is carry out in collaboration with Dr. Jaume Coll from the National Ceramic and Luxurious Arts Museum 'Gonzalez Marti'. - Reconstruction of the original tonality of blue degraded smalts on canvas from the measurement of the relationship of Co/Pb. - Analyses and comparative studies of engravings elaborated with different techniques (etching and heliogravure) from the XVII - XX centuries, and EDXRF analysis of ancient and currently commercialised inks. This project is developed in collaboration with Dr. Rosa Vives from the Barcelona University. - Identification and characterization of forged works of art. - In the near future: quantitative and semi-quantitative multi-element microanalysis of solid and liquid samples by TXRF. (author)

  10. X-ray fluorescence analysis of titanium alloys.

    Vassilaros, G L; McKaveney, J P

    1969-02-01

    An X-ray solution method is proposed for determining major amounts of Mo, Sn and Zr in Ti alloys. The method utilizes adjacent elements in the periodic table as internal standards and has been successfully applied to levels of 3-10% Sn, 11-40% Mo and 6-20% Zr. The procedure involves three steps: dissolving the sample with a suitable acid mixture; adding the suitable internal standard at the concentration levels experimentally found to give optimum accuracy and precision; analysing the resulting solution mixture by X-ray fluorescence. Antimony was found to be a suitable internal standard for its adjacent element tin at a concentration ratio of 3:1 Sb:Sn. Niobium was successfully used for both its adjacent elements, molybdenum and zirconium, at 2:1 concentration ratios, Nb:Mo and Nb:Zr. A number of elements non-adjacent to tin, molybdenum and zirconium (i.e., copper, bromine, titanium, bismuth and tantalum) were experimentally found unsuitable as internal standards. Concentration factors of the internal standard and the adjacent elements sought were found to affect significantly the precision of analysis. PMID:18960488

  11. X-ray fluorescence in IAEA Member States: Sri Lanka

    Full text: The Energy Dispersive X-ray Fluorescence (ED-XRF) facility was established in 2001 under the Technical Cooperation project on Development and Utilization of Nuclear Analytical Technology (SRL/2/005). The XRF facility consists of X-ray tube with Mo anode, secondary targets and Si/Li detector coupled with portable inspector MCA and Genie 2000 spectrum acquisition software. Qualitative and Quantitative analysis is being carried out using QXAS-BFP (Backscatter Fundamental Parameter method) for thick samples, QAES (P.Kump, Slovenia) for both intermediate thickness and thin samples. The EDXRF facility is used for the elemental analysis of soil /sediments samples, plant materials, air filters, alloys and water samples. The analytical services are provided for research institutions, Universities, Geological and Environmental assessment companies to determine major, minor and trace elements in various materials. Since 1998 the XRF group has also participated in the IAEA/RCA project on Isotopes and related techniques to assess Air Pollution. Currently, three research projects on the application of EDXRF technique in environmental studies are being carried out (author)

  12. Analysis of tungsten carbides by X-ray fluorescence spectrometry.

    Kinson, K; Knott, A C; Belcher, C B

    Five sample presentation techniques were examined for the X-ray fluorescence spectrometric analysis of tungsten carbide alloys in powder and cemented forms. Powder samples may be oxidized by air at 600 degrees before fusion (I), or preferably by lithium nitrate during fusion (II); the fusion is effected with lithium-lanthanum tetraborate followed by briquetting with graphite. Powder samples may also be blended with wax and briquetted (III). Cemented carbides are surface-prepared with silicon carbide before analysis (V). Briquettes prepared by blending carbide powder, lithium-lanthanum tetraborate and graphite (IV), give poor reproducibility, however, owing to micro-absorption effects the technique is not recommended. The determination of eight common elements in tungsten carbide is discussed and the relative standard deviations are 0.002-0.004 for major and 0.008-0.01 for minor elements. PMID:18961988

  13. Extraction-X-ray fluorescence determination of selenium

    Easy to use, rapid x-ray fluorescence method of selenium determination is developed. The method is based on preliminary extraction of Se with dithiophosphoric acid and evaporation of the extract on a porous matrix. To choose the optimal conditions of extraction the effect of organic reagent concentration, of the pH aqueous phase and the shaking up time on selenium extraction volume is studied. Selenium quantitative extraction is observed in the process of selenium extraction from highly acid media. It is shown that the optimal conditions for Se(4) extraction by means of ammonium diethyldithiophosphate are the following: reagent concentration is 1x10-3 M; pH 0-1.5; the shaking up time is 20 min. The given methods are applied for selenium determination in the bottoms the formations of the Noksa river. The absolute detection limit is 0.1 μg

  14. Using X-ray Fluorescence to Date Petroglyphs

    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.

  15. Laboratory micro-X-ray fluorescence spectroscopy instrumentation and applications

    Haschke, Michael

    2014-01-01

    Micro-X-ray fluorescence offers the possibility for a position- sensitive and non-destructive analysis that can be used for the analysis of non-homogeneous materials and layer systems. This analytical technique has shown a dynamic development in the last 15 years and is used for the analysis of small particles, inclusions, of elemental distributions for a wide range of different applications both in research and quality control. The first experiments were performed on synchrotrons but there is a requirement for laboratory instruments which offers a fast and immediate access for analytical results. The book discuss the main components of a µ-XRF instrument and the different measurement modes, it gives an overview about the various instruments types, considers the special requirements for quantification of non-homogeneous materials and presents a wide range of application for single point and multi-point analysis as well as for distribution analysis in one, two and three dimensions.

  16. X-ray fluorescence in IAEA Member States: Slovenia

    Full text: Research and development activities include: - development of quantification software for radioisotope and tube excited X-ray fluorescence spectrometry, based on use of fundamental parameters and emission-transmission method; - development of sensitive XRF technique for aerosol analysis, utilising excitation at small incident angles; - development of fast semi-quantitative analysis of samples in powder form by TXRF; - designing and manufacturing of portable XRF systems with radioisotope and tube excitation for use in archaeometry and for the analysis of pigments on paintings. Applications: - analysis of geological samples (geochemistry applications); - determination of P, S, Cl, K, Ca and some heavy metals in animal food (hay, grass silage and maize silage); - routine aerosol analysis in urban areas close to industrial facilities; - analysis of pigments from old paintings and other artefacts by TXRF; - analysis of vines and bee honey for the contents of S and some heavy metals by TXRF; - analysis of thin layers (Ti, Cr, Ni, and Zn ) used for anticorrosion protection. (author)

  17. Uranium concentrate analysis by X-ray fluorescence spectroscopy

    The determination of As, Ca, Fe, Mo, P, S, Si. Th, V and U in uranium concentrates by X-ray fluorescence spectroscopy has been studied. As and U are determined in nitric solutions and for the rest of elements analysis is performed by a bead fusion technique using Li2B4O7 and Li2CO3 as fluxes. Although the uranium matrix minimizes the absorption and enhancement effects, because of the content variations of this element it is advisable to operate at a constant level of U3O8. Despite the high matrix absorption and the large dilution of the samples, sensitivity and speed are found to be satisfactory as the result of the use of a high sensitivity automatic spectrometer. The spectral interferences of Mo on S and P, and of Pb on As have been particularly considered. (author)

  18. Environmental studies in Khartoum area using x-ray fluorescence

    In the present work an attempt has been made for the analysis of some soil, plant, sediments and fish samples of relevance to environmental pollution in Khartoum area. These samples have been collected from different places in residential areas, so as to cover industrial areas, agricultural and residential areas, as well as Tuti Island as control area. Special attention has been dedicated to the analysis of lead concentrations resulting from automobile-emissions in soils and to other toxic metals such as Cr in some industries. The samples were analysed by x-ray fluorescence (XRF) technique. The results obtained using XRF measurements and computer software called QXAS for data analysis. The concentrations of lead and some heavy metals such as Cr in soils from certain locations were alarming and may create pollution problems in the near future. The results obtained from different countries. The results are generally lower than the international limits. (Author)

  19. Determination of thorium by fluorescent x-ray spectrometry

    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.

  20. Analysis of solar blocker through portable X-ray fluorescence

    This paper estimates the concentration of TiO2 by Energy Dispersion X-ray fluorescence (EDXRF) viewing t obtain the FPS due to the physical barrier in the composition of solar blockers, and identifies possible present metals in the samples. A portable EDXRF equipment was used and 27 commercial of different brands and solar protection factors were analysed. Also, three formulations (A, B and C) were prepared and measured estimated in FPS-30 using 5% or TiO2. The quantification was performed through calibration curves with 1% to 30% standards of TiO2. As result, it was possible to determine the contribution to physical protection in the FPS, associated to the Ti concentration present in some solar blocker samples available in the market. Also, it was possible to detect the presence of various metals in solar protectors, such as Fe, Zn, Br and Sr, and identify chemical elements which were not mentioned and their formulation as well

  1. X-ray fluorescence beamline at LNLS: components and some associated techniques

    Perez, CArlos A.; Radtke, Martin; Perez, Carlos; Tolentino, Helio; Vicentin, Flavio [Laboratorio Nacional de Luz Sincrotron (LNLS), Campinas, SP (Brazil); Sanchez, Hector Jorge; Perez, Roberto D. [Universidad Nacional, Cordoba (Argentina). Facultad de Matematica, Astronomia y Fisica

    1997-12-31

    Full text. In this work a general description of the Total Reflection X-Ray Fluorescence (TXRF) and the X-Ray Fluorescence Microprobe (XRFM) is presented. Components, equipment and experimental stations for the x-ray fluorescence beamline are described, regarding to the techniques mentioned above. Results from the simulations of a pair bended mirrors in a Kirkpatrick-Baez configuration, are shown. The simulations were performed with Shadow program. (author)

  2. X-ray fluorescence beamline at LNLS: components and some associated techniques

    Full text. In this work a general description of the Total Reflection X-Ray Fluorescence (TXRF) and the X-Ray Fluorescence Microprobe (XRFM) is presented. Components, equipment and experimental stations for the x-ray fluorescence beamline are described, regarding to the techniques mentioned above. Results from the simulations of a pair bended mirrors in a Kirkpatrick-Baez configuration, are shown. The simulations were performed with Shadow program. (author)

  3. Direct comparison of soft x-ray images of organelles with optical fluorescence images

    Soft x-ray microscopes operating in the water window region are capable of imaging living hydrated cells. Up to now, we have been able to take some soft x-ray images of living cells by the use of a contact x-ray microscope system with laser produced plasma soft x-ray source. Since the soft x-ray images are different from the optical images obtained with an ordinary microscope, it is very important to identify what is seen in the x-ray images. Hence, we have demonstrated the direct comparison between the images of organelles obtained with a fluorescence microscope and those with a soft x-ray microscope. Comparing the soft x-ray images to the fluorescence images, the fine structures of the organelles could be identified and observed. (author)

  4. Azimuthal anisotropy of the scattered radiation in grazing incidence X-ray fluorescence

    Das, Gangadhar, E-mail: gdas@rrcat.gov.in; Tiwari, M. K.; Singh, A. K.; Ghosh, Haranath [Indus Synchrotrons Utilisation Division, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India)

    2015-06-24

    The Compton and elastic scattering radiations are the major contributor to the spectral background of an x-ray fluorescence spectrum, which eventually limits the element detection sensitivities of the technique to µg/g (ppm) range. In the present work, we provide a detail mathematical descriptions and show that how polarization properties of the synchrotron radiation influence the spectral background in the x-ray fluorescence technique. We demonstrate our theoretical understandings through experimental observations using total x-ray fluorescence measurements on standard reference materials. Interestingly, the azimuthal anisotropy of the scattered radiation is shown to have a vital role on the significance of the x-ray fluorescence detection sensitivities.

  5. X-ray fluorescence in IAEA Member States: Venezuela

    study on an in-situ microwave digestion prior to analysis of biological samples by total reflection X-ray fluorescence, Spectrochim. Acta 56B (2001) 2187-2194. L.M.Marco P., E. Jimenez, E.A. Hernandez C., A. Rojas and E.D.Greaves, Determination of Zn/Cu ratio and oligoelements in serum samples by total reflection X-ray fluorescence spectrometry for cancer diagnosis, Spectrochim. Acta 56B (2001) 2195-2202. J.I. Bermudez, E.D.Greaves. P. Nemeth and L. Sajo-Bohus, Determination of Technetium by total reflection X-ray fluorescence, Spectrochim. Acta 56B (2001) 2247-2252. L. Bennun, E.D. Greaves and J.J. Blostein, New procedure for intensity and detection limit determination in spectral trace analysis: application for trace mercury by TXRF, Accepted for publication in X-ray Spectrometry (2002). (author)

  6. Quo Vadis total reflection X-ray fluorescence?

    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 108 to 1014 [atoms/cm2] 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 1x1011 and 1x107 [atoms/cm2] 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 109 [atoms/cm2]. Novel detectors such as silicon drift detectors (SDD) with an active area of 5 mm2, 10 mm2 or 20 mm2, respectively, and multi-array detectors forming up to 70 mm2 are commercially available. The first SDD with 100 mm2 (!) 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

  7. X-ray fluorescence in IAEA Member States: Spain

    Full text: Instrumental facilities of the ICMUV include: a total reflection X ray fluorescence (TXRF) spectrometer, and laboratory and portable energy-dispersive X ray fluorescence (EDXRF) spectrometer. These instruments are applied in the field of art and archaeometry. Current projects are in collaboration with the Department of Prehistory and Archaeology (University of Valencia), the Valltorta Museum and Vetraria Munoz de Pablos S.L. In situ analysis of rock art painting by portable EDXRF spectrometry in the Valltorta Valley, East of Spain: A purpose of the research was to investigate the elemental composition of the prehistoric cave paintings located in the Valltorta Valley in Coves de Vinroma (Castellon, Spain) and to demonstrate the usefulness of portable EDXRF spectroscopy for in situ elemental analysis. Analysis of the red and black pigments by portable EDXRF showed the presence of iron and manganese compounds, respectively; in the future it will facilitate sampling decisions prior to use of other analytical methods to obtain additional information about chemical composition, structure and preparation techniques. Application of portable EDXRF system to the study of ancient glasses: Since there is no method available to determine directly the age of glass objects, it is necessary to compare the material composition of questionable pieces with genuine pieces. Therefore, a non-destructive and sensitive analytical technique was needed with a capability to perform in-situ measurements in order to avoid transportation of precious and fragile objects to the analytical laboratory. A portable EDXRF system meets these requirements more than adequately. The application of a portable XRF spectrometer for solving authenticity-related problems in the field of ancient glasses has demonstrated its capability for revealing essential information for study of the Stained Glass Windows of Avila Cathedral. During the restoration work, clear differences in the composition of

  8. A Versatile Field Instrument for X-Ray Fluorescence Analysis

    A portable X-ray fluorescence analyser has been developed consisting essentially of an Xe/CH4 proportional counter probe and an electronic unit with single-channel analyser, binary scaler, digital-to-analogue converter with meter- readout and an automatic gain control circuitry. The instrument utilizes the high energy resolution of proportional counters combined with the excellent long-term stability provided by automatic gain control (AGC). The radioactive source, 241Am, is suitable for the excitation of fluorescence X-rays in a wide range of elements, i.e. from Cr-K (Z = 24) to Tm-K (Z = 69) and from Ba-L (Z = 56) to U-L (Z = 92). The same source is simultaneously used for the AGC operation by measuring a small fraction of the 241Am gamma- radiation(59.6 keV) directly incident through a small collimator hole into the detector. The count-rate measured above a threshold at 57 keV, which is not affected by any other fluorescent or scattered radiation, is used to control the detector high voltage in order to obtain a constant energy calibration and to eliminate any drift of the detector and the electronics. Thus several fixed single-channel windows selected by a rotary switch can be set for various elements of interest. Once having been set in the laboratory no further calibration is necessary for field operation. The prototype of the instrument was originally developed and used to determine nickel coatings on steel, which necessitates a very high energy resolution of the detector. Without using filters a sufficient sensitivity could be obtained. The same probe can also be equipped with balanced filters and the electronic unit with a reversible scaler providing direct indication of the difference counting rate of the meter, without fluctuations. However, in many cases filters can be saved because of the high energy resolution of the detector. The design features of the instrument make it extremely suitable for a wide range of prospecting and mining applications

  9. Fast x-ray fluorescence microtomography of hydrated biological samples.

    Enzo Lombi

    Full Text Available Metals and metalloids play a key role in plant and other biological systems as some of them are essential to living organisms and all can be toxic at high concentrations. It is therefore important to understand how they are accumulated, complexed and transported within plants. In situ imaging of metal distribution at physiological relevant concentrations in highly hydrated biological systems is technically challenging. In the case of roots, this is mainly due to the possibility of artifacts arising during sample preparation such as cross sectioning. Synchrotron x-ray fluorescence microtomography has been used to obtain virtual cross sections of elemental distributions. However, traditionally this technique requires long data acquisition times. This has prohibited its application to highly hydrated biological samples which suffer both radiation damage and dehydration during extended analysis. However, recent advances in fast detectors coupled with powerful data acquisition approaches and suitable sample preparation methods can circumvent this problem. We demonstrate the heightened potential of this technique by imaging the distribution of nickel and zinc in hydrated plant roots. Although 3D tomography was still impeded by radiation damage, we successfully collected 2D tomograms of hydrated plant roots exposed to environmentally relevant metal concentrations for short periods of time. To our knowledge, this is the first published example of the possibilities offered by a new generation of fast fluorescence detectors to investigate metal and metalloid distribution in radiation-sensitive, biological samples.

  10. Experimental demonstration of direct L-shell x-ray fluorescence imaging of gold nanoparticles using a benchtop x-ray source

    Manohar, Nivedh; Reynoso, Francisco J.; Cho, Sang Hyun

    2013-01-01

    Purpose: To develop a proof-of-principle L-shell x-ray fluorescence (XRF) imaging system that locates and quantifies sparse concentrations of gold nanoparticles (GNPs) using a benchtop polychromatic x-ray source and a silicon (Si)-PIN diode x-ray detector system.

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

    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. - Hihglights: • The performance of the confocal micro X-ray fluorescence was studied. • Confocal micro X-ray fluorescence was used for identifying paint layers. • The multilayered paint fragments of a car were analyzed nondestructively

  12. Investigation of a tabletop confocal micro X-ray fluorescence setup

    A new tabletop confocal micro x-ray fluorescence setup with an MCBM 50-0.6B x-ray tube is assembled. The confocal micro x-ray fluorescence setup includes two lenses, a polycapillary full lens in the excitation channel and a polycapillary half lens in the detection channel. A Ni-Cr wire in diameter 25 μm is used to investigate the FWHM of three-dimensional confocal volume, A basso-relievo capital letter of a 1-jiao RMB coin of 2005 version is studied with this confocal micro x-ray fluorescence setup. (authors)

  13. X-ray fluorescence in IAEA Member States: Argentina

    Full text: The following projects carried out by the XRF Group are described: 1. Iridium Detection by Total Reflection x-Ray Fluorescence in Samples Providing from The Cretaceous-Tertiary Boundary and Experimental Amphibian Embryos - The main purpose of this study is to report the high sensitivity of TXRF for Ir measurements in mineral and biological samples. Mineral samples originate from different horizon deposits in the Neuquen basin, Argentina. Ir anomaly seems to be related to diderophite material provided to Earth in large quantities most probably by a 10 km asteroid that impacted earth 65 Myears ago. Sample preparation procedures and multielemental information are available. In a particular case of amphibian embryos, the detected level of Ir was in the order of 1 part per million (bioconcentration factor of 9). 2. Polymer Solutions on Glass: Adsorption Study by Total Reflection x-Ray Fluorescence - Equilibrium properties of a polymer solution in the vicinity of a solid-liquid interface are locally altered relative to the properties in bulk. This is caused probably by attractive or repulsive interactions adsorbed fraction-adsorbent. In this way, theoretical models for flexible and rod-like polymers were published.The present work is related to study of the adsorption of 0 to 0.05% aqueous scleroglucan solution on 400 to 600 μm glass microspheres. This study was possible by labeling the macromolecule by means of a chemical reaction with iodine, and then detecting by TXRF. Results show that for dilute concentration polymers behave in an anomalous way near the interface, contrary to the previous theoretical predictions. A first attempt to explain this behavior is presented. 3. Total Reflection x-Ray Fluorescence Polymer Spectra: Classification By Taxonomy Statistic Tools - The aim of this work is to explore the use of chemometric tools for the classification of synthetic and natural polymers with a mean molecular weight greater than 106. Spectra obtained by

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

    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.

  15. X-ray fluorescence in Member States: Argentina. Synchrotron radiation total reflection X-ray fluorescence study of gums

    Full text: Over the years, the term gums has been used for a wide range of compounds including polysaccharides, terpenes, proteins, and synthetic polymers. In the 1990s, the term more specifically denotes a group of industrially useful polysaccharides or their derivatives that hydrate in hot or cold water to form viscous solutions, dispersions, or gels. Gums are used in industry because their aqueous solutions or dispersions have suspending and stabilizing properties. In addition, gums may produce gels or act as emulsifiers, adhesives, flocculants, binders, film formers, lubricants, or friction reducers, depending on the shape and chemical nature of the particular gum. They have increasingly been used in recent years by industry due to their controlled, reproducible and economical biosynthesis, and their biodegradability. Gums are classified as natural or modified. Natural gums include seaweed extracts, plant exudates, gums from seed or root, and gums obtained by microbial fermentation. Modified (semi-synthetic) gums include cellulose and starch derivatives and certain synthetic gums such as low methoxyl pectin, propylene glycol alginate, and carboxymethyl and hydroxypropyl guar gum. Selected polymers from the different groups were characterised in this work. Specifications of these polymers have to be controlled by European Community, Mercosur, etc. especially for toxic metals in food and pharmaceutical products. Synchrotron Radiation (SR) induced Total Reflection X-ray Fluorescence (SRTXRF) analysis expands the possibilities of conventional TXRF based on X-ray tube excitation. In this study the SRTXRF technique was successfully applied for the quantification of F, Na, Mg, S, K, Ca, V, Cr, Mn, Fe, Ni, Cu, Zn, As and Pb in high-viscosity gum aqueous solutions. The results were analysed from both toxic and alimentary point of view. (author)

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

    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

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

    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

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

    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.

  19. A Brazilian tree collection analyzed by X ray fluorescence

    The analysis of the inorganic components of wood is of great interest for several reasons, including the acquisition of basic data creating a data base of values for individual species. Knowing the wide variability in matrix composition (lignin, oil, resin, silica) and densities (0.39-1.09 g cm-3), 40 species of trees were analysed by X ray fluorescence (XRF) to determine the concentrations of Br, Ca, Cu, K, Mn, Pb, Rb, Sr, and A. This technique is widely used because of its accuracy and simplicity of sample preparation, normally complex for this type of biological material. This multi-elemental analysis has proven suitable for wood, a material in which a wide range for each element was encountered in the different species studied: 0.3-5.2 for Br, 126-9074 for Ca, 2.2-11 for Cu, 108-5873 for K, 3.1-134 for Mn, 0.5-4.7 for Pb, 0.3-20 for Rb, 1.2-120 for Sr, and 1.1-20 for Zn (values given in μg g-1). (author)

  20. Pinhole X-ray Fluorescence Imaging of Gadolinium Nanoparticles: A Preliminary Monte Carlo Study

    Jung, Seong Moon; Sung, Won Mo; Ye, Sung Joon [Seoul National University, Seoul (Korea, Republic of)

    2014-10-15

    X-ray fluorescence imaging is a modality for the element-specific imaging of a subject through analysis of characteristic x-rays produced by exploiting the interaction of high atomic number elements and incoming x-rays. Previous studies have utilized a polychromatic x-ray source to investigate the production of in vivo x-ray fluorescence images for the assessment of concentrations and locations of gold nanoparticles. However, previous efforts have so far been unable to detect low concentrations, such as 0.001% gold by weight, which is an expected concentration accumulated in tumors. We examined the feasibility of a monochromatic synchrotron x-rays implementation of pinhole x-ray fluorescence imaging by Monte Carlo simulations using MCNP5. In the current study, gadolinium (Gd) nanoparticles, which have been widely used as a contrast agent in magnetic resonance imaging and also as a dose enhancer in radiation therapy, were chosen for tumor targeting. Since a monochromatic x-ray source is used, the increased x-ray fluorescence signals allow the detection of low concentrations of Gd. Two different monochromatic x-ray beam energies, 50.5 keV near the Kedge energy (i.e., 50.207 keV) of Gd and 55 keV, were compared by their respective imaging results. Using Monte Carlo simulations the feasibility of imaging low concentrations of Gd nanoparticles (e.g., 0.001 wt%) with x-ray fluorescence using monochromatic synchrotron x-rays of two different energies was shown. In the case of imaging a single Gd column inserted in the center of a water phantom, the fluorescence signals from 0.05 wt% and 0.1 wt% Gd columns irradiated with a 50.5 keV photon beam were higher than those irradiated with 55 keV. Below 0.05 wt% region no significant differences were found.

  1. Pinhole X-ray Fluorescence Imaging of Gadolinium Nanoparticles: A Preliminary Monte Carlo Study

    X-ray fluorescence imaging is a modality for the element-specific imaging of a subject through analysis of characteristic x-rays produced by exploiting the interaction of high atomic number elements and incoming x-rays. Previous studies have utilized a polychromatic x-ray source to investigate the production of in vivo x-ray fluorescence images for the assessment of concentrations and locations of gold nanoparticles. However, previous efforts have so far been unable to detect low concentrations, such as 0.001% gold by weight, which is an expected concentration accumulated in tumors. We examined the feasibility of a monochromatic synchrotron x-rays implementation of pinhole x-ray fluorescence imaging by Monte Carlo simulations using MCNP5. In the current study, gadolinium (Gd) nanoparticles, which have been widely used as a contrast agent in magnetic resonance imaging and also as a dose enhancer in radiation therapy, were chosen for tumor targeting. Since a monochromatic x-ray source is used, the increased x-ray fluorescence signals allow the detection of low concentrations of Gd. Two different monochromatic x-ray beam energies, 50.5 keV near the Kedge energy (i.e., 50.207 keV) of Gd and 55 keV, were compared by their respective imaging results. Using Monte Carlo simulations the feasibility of imaging low concentrations of Gd nanoparticles (e.g., 0.001 wt%) with x-ray fluorescence using monochromatic synchrotron x-rays of two different energies was shown. In the case of imaging a single Gd column inserted in the center of a water phantom, the fluorescence signals from 0.05 wt% and 0.1 wt% Gd columns irradiated with a 50.5 keV photon beam were higher than those irradiated with 55 keV. Below 0.05 wt% region no significant differences were found

  2. X-ray fluorescence in IAEA Member States: Spain

    Full text: Instrumental facilities of the ICMUV include: a Total-reflection X-Ray Fluorencence (TXRF), a static and a portable Energy Dispersive X-Ray Fluorescence (EDXRF) spectrometers. These equipments are employed in the field of the art and archaeometry, and some applications in this area are implemented. The portable EDXRF spectrometer is advisable to perform 'in situ' and on-line analysis in a multidisciplinary environment, the static EDXRF equipment is good to perform analysis on paper and metal pieces. The TXRF spectrometry is the best technique for very sensitive analysis of trace elements in microsamples. Using the last technique we have analyzed the cottons used by the restorers in the different steps of the restoration process; it appeared that the method is a good tool to study the composition of different layers and zones of the work of art. Current projects include: 1. Analysis of valuable antique ceramics that can be investigated only when the analysis does not result in any damage. EDXRF measurements with portable instrumentation provide non-destructive analysis that completely eliminates sampling. An alternative method to determine the overglaze or underglaze pigment decoration is the microscopic examination of a ceramic cross section, but this examination requires sampling and damage to the physical integrity of the object. The aim of our work is to apply nondestructive technique ensuring the physical integrity of the object. We have proposed a portable EDXRF spectrometer to identify the underglaze and overglaze pigment decoration of ceramics on the basis of different values for the ratio between the Pb(Lα) line from the main element of the glaze cover and the Kα lines from the main elements (Co, Mn, Ni) found in the pigment, when the angle of the incidence radiation is varied. If the position of the detector is fixed, these ratios (Pb(Lα)/Co(Kα), etc.) increases with the angle for underglaze decoration, and decreases for overglaze decoration

  3. Quantitative x-ray fluorescence analysis using monochromatic synchrotron radiation

    The use of high-intensity, tunable monochromatic x-rays for the quantitative analysis of biological and geochemical specimens at the 10-8 g level is described. Incident x-rays were obtained from the new LBL-EXXON permanent magnet wiggler beamline at the Stanford Synchrotron Radiation Laboratory. The sample detector geometry was designed to make optimal use of polarization advantages for background reduction. Questions regarding the sensitivity and accuracy of the measurements were studied with particular emphasis on the advantages of tuning the x-ray energies for optimum excitation for specific elements. The implications of these measurements with respect to the use of x-ray microprobe beams will be discussed

  4. Romanian medieval earring analysis by X-ray fluorescence technique

    Therese, Laurent; Guillot, Philippe, E-mail: philippe.guillot@univ-jfc.fr [Laboratoire Diagnostics des Plasmas, CUFR J.F.C, Albi (France); Muja, Cristina [Laboratoire Diagnostics des Plasmas, CUFR J.F.C, Albi (France); Faculty of Biology, University of Bucharest (Romania); Vasile Parvan Institute of Archaeology, Bucharest, (Romania)

    2011-07-01

    Full text: Several instrumental techniques of elemental analysis are now used for the characterization of archaeological materials. The combination between archaeological and analytical information can provide significant knowledge on the constituting material origin, heritage authentication and restoration, provenance, migration, social interaction and exchange. Surface mapping techniques such as X-Ray Fluorescence have become a powerful tool for obtaining qualitative and semi-quantitative information about the chemical composition of cultural heritage materials, including metallic archaeological objects. In this study, the material comes from the Middle Age cemetery of Feldioara (Romania). The excavation of the site located between the evangelical church and the parsonage led to the discovery of several funeral artifacts in 18 graves among a total of 127 excavated. Even if the inventory was quite poor, some of the objects helped in establishing the chronology. Six anonymous Hungarian denarii (silver coins) were attributed to Geza II (1141-1161) and Stefan III (1162-1172), placing the cemetery in the second half of the XII century. This period was also confirmed by three loop shaped earrings with the end in 'S' form (one small and two large earrings). The small earring was found during the excavation in grave number 86, while the two others were discovered together in grave number 113. The anthropological study shown that skeletons excavated from graves 86 and 113 belonged respectively to a child (1 individual, medium level preservation, 9 months +/- 3 months) and to an adult (1 individual). In this work, elemental mapping were obtained by X-ray fluorescence (XRF) technique from Jobin Yvon Horiba XGT-5000 instrument offering detailed elemental images with a spatial resolution of 100{mu}m. The analysis revealed that the earrings were composed of copper, zinc and tin as major elements. Minor elements were also determined. The comparison between the two

  5. Romanian medieval earring analysis by X-ray fluorescence technique

    Full text: Several instrumental techniques of elemental analysis are now used for the characterization of archaeological materials. The combination between archaeological and analytical information can provide significant knowledge on the constituting material origin, heritage authentication and restoration, provenance, migration, social interaction and exchange. Surface mapping techniques such as X-Ray Fluorescence have become a powerful tool for obtaining qualitative and semi-quantitative information about the chemical composition of cultural heritage materials, including metallic archaeological objects. In this study, the material comes from the Middle Age cemetery of Feldioara (Romania). The excavation of the site located between the evangelical church and the parsonage led to the discovery of several funeral artifacts in 18 graves among a total of 127 excavated. Even if the inventory was quite poor, some of the objects helped in establishing the chronology. Six anonymous Hungarian denarii (silver coins) were attributed to Geza II (1141-1161) and Stefan III (1162-1172), placing the cemetery in the second half of the XII century. This period was also confirmed by three loop shaped earrings with the end in 'S' form (one small and two large earrings). The small earring was found during the excavation in grave number 86, while the two others were discovered together in grave number 113. The anthropological study shown that skeletons excavated from graves 86 and 113 belonged respectively to a child (1 individual, medium level preservation, 9 months +/- 3 months) and to an adult (1 individual). In this work, elemental mapping were obtained by X-ray fluorescence (XRF) technique from Jobin Yvon Horiba XGT-5000 instrument offering detailed elemental images with a spatial resolution of 100μm. The analysis revealed that the earrings were composed of copper, zinc and tin as major elements. Minor elements were also determined. The comparison between the two large earrings

  6. Measurement uncertainty in Total Reflection X-ray Fluorescence

    Total Reflection X-ray Fluorescence (TXRF) spectrometry is a multi-elemental technique using micro-volumes of sample. This work assessed the components contributing to the combined uncertainty budget associated with TXRF measurements using Cu and Fe concentrations in different spiked and natural water samples as an example. The results showed that an uncertainty estimation based solely on the count statistics of the analyte is not a realistic estimation of the overall uncertainty, since the depositional repeatability and the relative sensitivity between the analyte and the internal standard are important contributions to the uncertainty budget. The uncertainty on the instrumental repeatability and sensitivity factor could be estimated and as such, potentially relatively straightforward implemented in the TXRF instrument software. However, the depositional repeatability varied significantly from sample to sample and between elemental ratios and the controlling factors are not well understood. By a lack of theoretical prediction of the depositional repeatability, the uncertainty budget can be based on repeat measurements using different reflectors. A simple approach to estimate the uncertainty was presented. The measurement procedure implemented and the uncertainty estimation processes developed were validated from the agreement with results obtained by inductively coupled plasma — optical emission spectrometry (ICP-OES) and/or reference/calculated values. - Highlights: • The uncertainty of TXRF cannot be realistically described by the counting statistics. • The depositional repeatability is an important contribution to the uncertainty. • Total combined uncertainties for Fe and Cu in waste/mine water samples were 4–8%. • Obtained concentrations agree within uncertainty with reference values

  7. X-ray fluorescence in IAEA Member States: Nigeria

    Full text: Environmental Research Laboratory (ERL) has got EDXRF system with total reflection module. These facilities are used for training, research and analytical services. Training is provided for Physics, Chemistry and Geology for both undergraduate and postgraduate students. The samples analysed in our laboratory include environmental, geological, biological, water, steel and alloy materials. The Research activities are carried out in support of environmental studies for air, water, soils and plant materials and optimisation of measurement protocols. We provides analytical services for the determination of major and minor elements in small-scale prospectors and miners of mineral ores with major constituents such as K, Ca, Ti, Cr, Mn, As, Pb and Zr. Presently we are monitoring environmental pollution due to toxic heavy metals in industrial workplaces. Other analytical services rendered by the laboratory include determination of trace elements in Nigerian bitumen samples, determination of toxic heavy metals like Ti, Cr, Mn, Fe, Cu, Zn, As, Pb, Cd, Hg in various stages of dam water in Ile-Ife- the university community. The laboratory also offered analytical services to other research institutions, Universities, governmental agencies, geological and environmental assessment companies. ERL group is currently participating in different projects/conferences organized by the International Atomic Energy Agency (IAEA), Vienna with the following papers presented: (1) Determination of atmospheric concentration of toxic metals along urban motorway in two Nigerian cities using TXRF technique (2) Assessment of Occupational Exposure to Toxic Metals in some Paint and Secondary Iron and Steel Industries in Lagos, Nigeria using TXRF Technique. One of the postgraduate projects already completed is on Determination of Concentration of Toxic Metals in the Ambient Air in Lagos and Ile-Ife, Nigeria, using Total Reflection X-ray Fluorescence Technique. (author)

  8. Measurement uncertainty in Total Reflection X-ray Fluorescence

    Floor, G.H., E-mail: geerke.floor@gfz-potsdam.de [GFZ German Research Centre for Geosciences Section 3.4. Earth Surface Geochemistry, Telegrafenberg, 14473 Postdam (Germany); Queralt, I. [Institute of Earth Sciences Jaume Almera ICTJA-CSIC, Solé Sabaris s/n, 08028 Barcelona (Spain); Hidalgo, M.; Marguí, E. [Department of Chemistry, University of Girona, Campus Montilivi s/n, 17071 Girona (Spain)

    2015-09-01

    Total Reflection X-ray Fluorescence (TXRF) spectrometry is a multi-elemental technique using micro-volumes of sample. This work assessed the components contributing to the combined uncertainty budget associated with TXRF measurements using Cu and Fe concentrations in different spiked and natural water samples as an example. The results showed that an uncertainty estimation based solely on the count statistics of the analyte is not a realistic estimation of the overall uncertainty, since the depositional repeatability and the relative sensitivity between the analyte and the internal standard are important contributions to the uncertainty budget. The uncertainty on the instrumental repeatability and sensitivity factor could be estimated and as such, potentially relatively straightforward implemented in the TXRF instrument software. However, the depositional repeatability varied significantly from sample to sample and between elemental ratios and the controlling factors are not well understood. By a lack of theoretical prediction of the depositional repeatability, the uncertainty budget can be based on repeat measurements using different reflectors. A simple approach to estimate the uncertainty was presented. The measurement procedure implemented and the uncertainty estimation processes developed were validated from the agreement with results obtained by inductively coupled plasma — optical emission spectrometry (ICP-OES) and/or reference/calculated values. - Highlights: • The uncertainty of TXRF cannot be realistically described by the counting statistics. • The depositional repeatability is an important contribution to the uncertainty. • Total combined uncertainties for Fe and Cu in waste/mine water samples were 4–8%. • Obtained concentrations agree within uncertainty with reference values.

  9. 3D micro-XRF for cultural heritage objects: new analysis strategies for the investigation of the Dead Sea Scrolls.

    Mantouvalou, Ioanna; Wolff, Timo; Hahn, Oliver; Rabin, Ira; Lühl, Lars; Pagels, Marcel; Malzer, Wolfgang; Kanngiesser, Birgit

    2011-08-15

    A combination of 3D micro X-ray fluorescence spectroscopy (3D micro-XRF) and micro-XRF was utilized for the investigation of a small collection of highly heterogeneous, partly degraded Dead Sea Scroll parchment samples from known excavation sites. The quantitative combination of the two techniques proves to be suitable for the identification of reliable marker elements which may be used for classification and provenance studies. With 3D micro-XRF, the three-dimensional nature, i.e. the depth-resolved elemental composition as well as density variations, of the samples was investigated and bromine could be identified as a suitable marker element. It is shown through a comparison of quantitative and semiquantitative values for the bromine content derived using both techniques that, for elements which are homogeneously distributed in the sample matrix, quantification with micro-XRF using a one-layer model is feasible. Thus, the possibility for routine provenance studies using portable micro-XRF instrumentation on a vast amount of samples, even on site, is obtained through this work. PMID:21711051

  10. [Methods of detector response function establishment in X-ray fluorescence spectra analysis].

    Li, Zhe; Tuo, Xian-Guo; Yang, Jian-Bo; Liu, Ming-Zhe; Cheng, Yi; Wang, Lei; Zhou, Jian-Bin

    2012-11-01

    During the measurement and analysis process of X-ray fluorescence spectra, it is very helpful to improve the analyze speed, accuracy and automaticity of X-ray fluorescence spectra analysis by establishing detector response function(DRF), which represents the shape of full energy peak and can provide former basic data for subsequent X-ray analysis technique. For the theory and model of semiconductor DRF in X-ray energy spectrum measurements, methods of three typical detector response function model establishment, key parameters of full energy peak standard deviation and Fano factor calculation, etc. are discussed, and meanwhile, the summarization and contrast of existing studies are shown in this paper. Finally, the suggestion for modeling methods of DRF in X-ray fluorescence spectra measurements is provided. PMID:23387190

  11. X-ray fluorescence in IAEA Member States: Albania

    Full text: The activities on Energy-Dispersive X-ray Fluorescence Laboratory at the Institute of Nuclear Physics (INP) in Tirana, Albania started about 30 years ago from using simple systems consisting of single channel analysers, radioisotope sources and gas proportional or scintillation counters along with balanced filters for the separation of analytical lines. These systems were applied for the determination of single elements. A few portable prototypes were developed and successfully used for the determination of chromium and copper in ores, both in the lab and institute (ore processing plants) conditions. Later, through different TC projects with IAEA, the lab has been equipped with the following systems: X-ray tube excited EDXRF spectrometer with secondary target excitation; radioisotope excited EDXRF system; TXRF module; field portable XRF system based on a Cd-109 disc source; Si-PIN detector and pocket MCA. From the beginning our work has been focused on research, applications and training. Due to the fact that our EDXRF systems are made of different parts that are put together, our research activities are mainly related to optimization of excitation geometry and the development of optimized analytical procedures for the analysis of different group of elements in several kinds of samples. Some of these procedures include: determination of major and minor elements in soils, sediments, mineral ores and different type of rocks; determination of sulphur and some trace elements (V, Ni, etc.) in oil, bitumen and asphaltene; determination of some trace metals in sea and surface waters; determination of elemental composition of aerosols loaded on filters; determination of some trace elements in biological samples. An important point of our work is related with the quality of the analytical results. For this reason we have participated in some of the intercomparison runs organized by AQCS of the IAEA and in the GeoPT proficiency tests. In most cases our reported

  12. Sampling, storage and sample preparation procedures for X ray fluorescence analysis of environmental materials

    X ray fluorescence (XRF) method is one of the most commonly used nuclear analytical technique because of its multielement and non-destructive character, speed, economy and ease of operation. From the point of view of quality assurance practices, sampling and sample preparation procedures are the most crucial steps in all analytical techniques, (including X ray fluorescence) applied for the analysis of heterogeneous materials. This technical document covers recent modes of the X ray fluorescence method and recent developments in sample preparation techniques for the analysis of environmental materials. Refs, figs, tabs

  13. Extraction x-ray fluorescence determination of scandium in technological solutions

    Combined extraction x-ray fluorescence method of scandium determination in technological solutions of metallurgy is suggested. 10-20 % mass solution of HDEHP in crude fraction of higher carboxylic acids (HCA) was used as extractant. Scandium is extracted completely by HCA-HDEHP melt even from acid solutions. This enables to extract it selectively from technological solutions. The prepared solid extracts represent finished targets for x-ray fluorescence analysis. It is shown that scandium determination by extraction x-ray fluorescence method enables to decrease the relatice standard deviation, improve rapidity of determination. The lower limit of determination - 0.001 %

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

    Trojek, Tomas [Department of Dosimetry and Application of Ionizing Radiation, Czech Technical University in Prague (Czech Republic)], E-mail: tomas.trojek@fjfi.cvut.cz; Hlozek, Matin [Department of Archaeology and Museology, Faculty of Arts, Masaryk University, Brno (Czech Republic); Cechak, Tomas; Musilek, Ladislav [Department of Dosimetry and Application of Ionizing Radiation, Czech Technical University in Prague (Czech Republic)

    2010-04-15

    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.

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

    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.

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

    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. PMID:19914840

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

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

  18. A POLYNOMIAL CORRECTION TECHNIQUE USING RhKα COMPTON PEAK IN X-RAY FLUORESCENCE SPECTROMETRY

    包生祥

    2003-01-01

    @@ Compton scattering radiation of an X ray tube target line is widely used for matrix absorption correction in X-ray fluorescence analysis of heavy trace elements in light matrix samples,Compton scatter ing internal standard technique has been a routine method in geological samples since Reynolds recommended the method in 1963.

  19. Determination of platinum in ores by a combined fire assay-X-ray fluorescence method

    A combined fire assay-X-ray fluorescence procedure for the determination of platinum in ores is described. Silver beads obtained by cupellation in the classical fire assay process are flattened to constant thickness before placement in the X-ray beam. A standard plot of platinum-silver intensity ratio versus platinum concentration is used to measure the platinum content of ore samples

  20. Microprocessor-based system for automatic X-ray diffraction and fluorescence

    A data acquisition and processing device appropriate for X-ray analysis and goniometer control was built. The Z-80 based system as well as the whole architeture is described. The advantages and new possibilities of the automated instrument as compared to the traditional ones are listed. The X-ray diffraction and fluorescence techniques can take advantage of the automation. (Author)

  1. X-ray fluorescence in IAEA Member States: Greece

    The Laboratory of Material Analysis (LMA) of the Institute of Nuclear Physics (INP) at the National Center for Scientific Research (NCSR) 'Demokritos', has been involved very actively during the past few years in the development, evaluation and analytical application of portable X-Ray Fluorescence (XRF) instruments, applied in particular for the non-destructive analysis of cultural materials. The study, conservation and preservation of cultural materials are considered nowadays issues of main concern for countries and international cultural organizations. Due to the strong interest and motivation from archaeologists, conservators and archaeometrical scientists in Greece and elsewhere, a large network has been developed involving the LMA and archaeologists/conservator scientists from Museums (Benaki Museum in Athens), Cultural Foundations (Thera Foundation P. Nomikos), the Greek Ministry of Culture-Conservation Department, Foreign Schools in Greece (American School of Classical Studies, French School of Athens), Universities (Department of Conservation of Antiquities and Works of Art in the Technological Educational Institution of Athens, University of Cincinnatti, Universite de Paris I, Pantheon Sorbonne), private sectors (THETIS, Thetis Authentics - Science and Techniques for Art History Conservation Ltd) and Institutions (Centre de Recherche et de Rastauration des Musees de France, LNS-INFN, LANDIS group). A variety of cultural materials/artifacts have been examined so far, including ceramic vases with colored decoration, bronze artifacts, wall-painting pigments, traces of polychromy on marble sculptures, Gold and Silver ancient jewelry, Gemstones, Roman Coins. Our research and analytical applications of the in-situ XRF analysis have been focused so far on the following: 1) optimum selection and integration of portable XRF instrumentation for improving analytical and sensitivity range; 2) evaluation of the potential of in-situ XRF analysis to provide specific

  2. X-ray fluorescence in IAEA Member States: Mongolia

    Full text: The Nuclear Research Center for Research and Training has got three EDXRF systems with isotopic sources (Cd-109, Am-241), secondary target and total reflection module. These facilities are used for training, research and analytical services. Training is provided for students of Physics and Chemistry at both undergraduate and postgraduate levels. The samples analyzed consist essentially of environmental, geological, biological, steel and alloy materials. Research activities are carried out in the areas of mineral resources and environmental studies (including analysis of air, water, biological and geological materials) and optimization of the measurement protocols. Since 1976 the Radioisotope EDXRF system has been used for the determination of major and minor elements in copper-molybdenum and polymetallic ores samples in support of effective exploitation of mineral resources. With Cd-109 excitation the Cu-Mo ores and tail samples are analyzed for the contents of major elements, such as Cr, Mn, Fe, Cu, Zn, As, Pb, Zr and Mo. With Am-241 excitation the Cu and Mo concentrates are analyzed for major elements such as Cu, Mo, Fe and minor toxic elements such as As, Sb and Ag. Since 1993 the TXRF system has been used for determination of toxic heavy metals (Ti, Cr, Mn, Fe, Cu, Zn, As, Pb, Cd, Hg) and other trace elements in water, alcohol, products of fermentation and food samples. This technique appeared to be extremely useful for environmental studies and pollution monitoring. The analytical services are provided for research institutions, universities, governmental agencies, geological and environmental assessment companies, prospectors and miners. Other analytical services include the determination of trace elements in soil, sediment and rock samples. The XRF group has also participated in different projects organized by the IAEA. Under a Coordinated Research Project (CRP) on 'In-situ Applications of X-Ray Fluorescence Techniques' a portable XRF analyzer

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

    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.

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

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

    2010-02-15

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

  5. Some application of the X-ray fluorescence by radioisotopic excitation on rocks and ores

    This work presents some principal concepts in which is founded the X-ray fluorescence, by radioisotopic stimulation technic. In the next itens the factors responsible by the introduction of the error in the dosage, and the analytical process are analysed. Some of possible applications of this methodology, principally in the mineral research, following this technique is compared with others analytical methods, including the conventional, X-ray fluorescence. (C.D.G.)

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

    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 HNO3/HClO4, mixing this solution with the internal standard and recording their Total Reflection X-ray Fluorescence spectra after calibration of the instrument. The results thus obtained were compared with those obtained by Inductively Coupled Plasma Mass Spectrometry and were found in good agreement. The average precision of the Total Reflection X-ray Fluorescence determinations was 5.5% (1σ) and the average deviation of Total Reflection X-ray Fluorescence determined values with that of Inductively Coupled Plasma Mass Spectrometry was 7.3%. These studies have shown that Total Reflection X-ray Fluorescence offers a promising and potential application in forensic work of this nature.

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

    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.

  8. ISS Ammonia Leak Detection Through X-Ray Fluorescence

    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

  9. Child lead exposure determined from measurement of x-ray fluorescence of teeth in situ

    X-ray fluorescence from lead when irradiated by gamma rays from a Co-57 source was utilized to measure the lead concentration in children's teeth in situ. The sensitivity of the method was adequate to detect 15 ppM from a gamma ray exposure to the tooth approximately 1/10 the exposure of a routine dental x-ray examination. The tooth lead levels assayed using x-ray fluorescence correlated well with chemical assay techniques for both extracted permanent and shed primary teeth. Thirty children from the Children's Hospital of Philadelphia suspected of having elevated lead levels had tooth lead levels measured in situ determined using the x-ray fluorescent technique. The tooth lead concentration varied from a low of 16 ppM to a high of 56 ppM

  10. Combined use of hard X-ray phase contrast imaging and X-ray fluorescence microscopy for sub-cellular metal quantification.

    Kosior, Ewelina,; Bohic, Sylvain; Suhonen, Heikki; Ortega, Richard; Devès, Guillaume; Carmona, Asuncion; Marchi, Florence; Guillet, Jean Francois; Cloetens, Peter

    2012-01-01

    Hard X-ray fluorescence microscopy and magnified phase contrast imaging are combined to obtain quantitative maps of the projected metal concentration in whole cells. The experiments were performed on freeze dried cells at the nano-imaging station ID22NI of the European Synchrotron Radiation Facility (ESRF). X-ray fluorescence analysis gives the areal mass of most major, minor and trace elements; it is validated using a biological standard of known composition. Quantitative phase contrast imag...

  11. Development of a portable system of X-ray fluorescence spectrometry

    This paper develops a compact and portable spectrometry system that will be used at the Laboratory of Applied Physics to the Biomedical and Environmental Sciences of the Institute of Physics/UERJ, Rio de Janeiro, Brazil. The laboratory both prepares the samples and develops the X-ray spectrometry techniques. The techniques of X-ray diffraction and fluorescence on various samples (biological, industrial and environmental) are used, attending to pos-graduation and graduation students, with multidisciplinary characteristics. The Mini-X system consists of X-ray mini tube MINI-X from Amptek with tungsten (W) target, and a compact spectrometer X123, also from Amptek that includes a detector, pre-amplifier, digital pulse processor, and multichannel. All the system is controlled by dedicated microprocessor. This work will present both a methodology for alignment and calibration of the system as far the first measurements performed using the X-ray fluorescence technique on standard samples. The multi elementary analysis by X-ray fluorescence (XRF) is based on the measurements of the characteristic X-ray intensity emitted by the chemical elements components of the samples when excited. Therefore, from the development of this compact and versatile system it will be possible to obtain the fluorescent intensities of the analysed samples at the Laboratory, not only at the research area but at the teaching area. Besides, new laboratory practices are being developed for the discipline of medical physics

  12. X-Ray Diffraction and X-Ray Fluorescent Analyses of Prehistoric Pottery Shards from Ulu Kelantan

    Zuliskandar Ramli

    2011-01-01

    Full Text Available Problem statement: X-Ray Diffraction (XRD and X-Ray Fluorescent (XRF were used in order to obtain mineralogical and elemental composition of seven pottery shards that have been unearthed during the excavation at Peraling Cave and Cha Cave in Ulu Kelantan, Malaysia. Approach: Peraling Cave and Cha Cave were prehistoric sites dating from 10, 000 BC which were inhabited by Hoabinhian people and then continuously used by people of Neolithic culture around 3000 BC. Results: Mineralogical and elemental analyses were carried out to determine whether the pottery found in the archaeological sites was locally made or trading items. Several clay samples from rivers in Ulu Kelantan such as Perias River, Chai River, Peralon River, Nenggiri River, Betis River and Jenera River were taken to be analysed. Conclusion/Recommendations: Mineralogical and elemental content of the pottery shards showed that the pottery shards did not originate from the Ulu Kelantan area and one of the samples contained clinochlore mineral. Clinochlore forms from the metamorphic and hydrothermal alterations of other iron and magnesium silicate minerals and is usually found in igneus rock and metamorphic rock formation.

  13. Cryo X-ray microscope with flat sample geometry for correlative fluorescence and nanoscale tomographic imaging.

    Schneider, Gerd; Guttmann, Peter; Rehbein, Stefan; Werner, Stephan; Follath, Rolf

    2012-02-01

    X-ray imaging offers a new 3-D view into cells. With its ability to penetrate whole hydrated cells it is ideally suited for pairing fluorescence light microscopy and nanoscale X-ray tomography. In this paper, we describe the X-ray optical set-up and the design of the cryo full-field transmission X-ray microscope (TXM) at the electron storage ring BESSY II. Compared to previous TXM set-ups with zone plate condenser monochromator, the new X-ray optical layout employs an undulator source, a spherical grating monochromator and an elliptically shaped glass capillary mirror as condenser. This set-up improves the spectral resolution by an order of magnitude. Furthermore, the partially coherent object illumination improves the contrast transfer of the microscope compared to incoherent conditions. With the new TXM, cells grown on flat support grids can be tilted perpendicular to the optical axis without any geometrical restrictions by the previously required pinhole for the zone plate monochromator close to the sample plane. We also developed an incorporated fluorescence light microscope which permits to record fluorescence, bright field and DIC images of cryogenic cells inside the TXM. For TXM tomography, imaging with multi-keV X-rays is a straightforward approach to increase the depth of focus. Under these conditions phase contrast imaging is necessary. For soft X-rays with shrinking depth of focus towards 10nm spatial resolution, thin optical sections through a thick specimen might be obtained by deconvolution X-ray microscopy. As alternative 3-D X-ray imaging techniques, the confocal cryo-STXM and the dual beam cryo-FIB/STXM with photoelectron detection are proposed. PMID:22273540

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

    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

  15. Automatic energy dispersive x-ray fluorescence analysing apparatus

    The invention discloses a number of improvements for an energy dispersive X-ray analysis system having computer supervised data collection, display and processing. The systems with which the improved circuitry and methods may be used include a dual interlocking bus structure so that the analyzer and computer functions communicate directly with each other and the user has immediate keyboard control of both. Such a system normally includes a system base control, a control console and a display console. The portions of the system which have been improved include a new type of ratemeter which gives a voltage output proportional to the intensity of the energy window or windows under consideration, an output which is an absolute digital representation of the intensity count rate, circuitry for input multiplexing and multiple output voltage buffering of the ratemeter to accomodate multiple single channel signals, and a new dead time correction to enable meaningful single channel intensity data to be handled by the system. An extension of the ratemeter is also disclosed for use in conjunction with X-ray mapping, enabling enhancements to be made on mapping SCA data

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

    Meira, Luiza L. C.; Inocente, Guilherme F.; Vieira, Leticia D.; Mesa, Joel [Departamento de Fisica e Biofisica - Instituto de Biociencias de Botucatu, Universidade Estadual Paulista Julio de Mesquita Filho (Brazil)

    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.

  17. X-ray fluorescence analysis of erbium oxide/oxalate for rare earth impurities

    A method for the determination of Tb, Dy, Ho, Tm, Yb, Lu and Y oxides in Er2O3 is described. 450 mg sample in the oxalate form is mixed with 150 mg boric acid binding material and pressed into a 1.25 inch diameter pellet over a supporting pellet of boric acid. The sample is then irradiated by X-rays from a tungsten tube and the fluorescent X-rays are dispersed by a LiF (200) crystal in a Philips PW 1220 semiautomatic X-ray fluorescence spectrometer. The intensities of characteristic X-rays of the impurity elements are measured by a flow proportional counter for all elements except yttrium for which the intensities are measured by a scintillation counter. The lowest determination limit is 0.005% for all impurities except for Yb for which it is 0.01%. Calculations for theoretical detection limit are given. (author)

  18. Synchrotron X-ray fluorescence analysis in environmental and earth sciences

    Adams F.

    2010-12-01

    Full Text Available Compared to other microscopic analytical tools X-ray microscopy techniques have the advantage that the large penetration depth of X-rays in matter allows one to investigate the interior of an object without destructive sample preparation. In combination with X-ray fluorescence tomography, analytical information from inside of a specimen can be obtained. Different X-ray analytical techniques can be used to produce contrast, X-ray absorption, fluorescence, and diffraction, to yield chemical, elemental, and structural information about the sample. Scanning microscopy on the basis of various lens systems in synchrotron radiation sources provides a routine spatial resolution of now about 100 nanometer but in the foreseeable future a 10–20 nanometer spatial resolution can be expected. X-ray absorption spectrometry can also provide chemical (speciation information on the sample. All this makes X-ray microscopy attractive to many fields of science. In this paper the techniques are briefly reviewed and a number of applications in the earth, planetary and cosmos sciences are illustrated with state-of-the art examples, while applications in the environmental sciences and biology are also briefly discussed.

  19. Analysis of uranium ores by energy dispersive X-ray fluorescence

    The determination of uranium in ores by energy-dispersive X-ray fluorescence (XFA) is demonstrated for uranium ore samples of known content. For calibration silica gel standards are used. Matrix effects are corrected by measuring the Compton scattering peaks. The radionuclide 109Cd as well as a X-ray tube in combination with Mo or Sn as secondary targets are suited as X-ray sources. The mean relative deviation of the values found from the given values is 5%. (orig.)

  20. A design of portable energy dispersive X-ray fluorescence analyzer

    A portable energy dispersive X-ray fluorescence analyzer (EDXRF) is designed. Excitation source is a small-caliber X-ray tube with Mo target. High-voltage power supply and filament supply is designed based on inverter technology. Semiconductor detectors is electric refrigerated, the qualities of the analyzer and the energy calibration curve are studied by the energy spectrum measurements for Cu, Zn, Ni, Pb, and the best range of elemental analysis is given by the theoretical analysis. (authors)

  1. Investigation of flour by X-ray fluorescence trace element analysis

    The determination of the trace element content of some kinds of flour by X-ray fluorescence analysis is described. The samples are burned to ashes at 700 deg C then calibration standards are added to them. The X-ray spectra are evaluated by computer. The optimal thickness of samples for achieving suitable accuracy and short measuring time is investigated. The trace element content of some species of Hungarian wheat is determined and compared. (D.Gy.)

  2. K X-ray fluorescent source for energy-channel calibration of the spectrometer

    2001-01-01

    A new K X-ray fluorescent source for calibrating the X or γ-ray multichannel analyzer spectrometer is introduced. A detailed description of the K fluorescent source device is given. The calibration method used and experimental results obtained are presented. The purity and efficiency of K fluorescence photons from this device are discussed. This new fluorescent source may be used as a substitute for radioactive nuclides for the energy-channel calibration of some MCA spectrometers.

  3. Comparison of different X-ray fluorescence analysis methods of total element content in soil

    Soil is a heterogeneous material and large variations in its chemical and physical nature can occur in a random samples collected in a small area of apparently similar land. Environmental analyses of soils call for rapid quantitative analysis techniques. X-ray fluorescence analysis has been used for many years and various sample preparation methods and analysis techniques have been used. Sample inhomogeneity is a very critical aspect of such a multielement analysis technique because rather small amount of soil generally are used for analyses. The aim of the current report is to compare different x-ray fluorescence techniques and sample preparation methods. Soil samples were collected from two different places in Botswana: Serowe and Gaborone.Three different x-ray fluorescence analysis techniques were used in the analysis of sandy soils. Two of them were energy-dispersive x-ray fluorescence spectrometers. The third was a total -reflection x-ray fluorescence spectrometer. A comparison shows that TXRF gives comparable results to EDXRF (second method). All results were within 10-15%. The conclusion is that TXRF is a suitable method not only for chemical speciation of soil, but also for the analysis of total fraction of elements

  4. Investigation of elemental distribution in lung samples by X-ray fluorescence microtomography

    X-Ray Fluorescence Microtomography (XRFCT) is a suitable technique to find elemental distributions in heterogeneous samples. While x-ray transmission microtomography provides information about the linear attenuation coefficient distribution, XRFCT allows one to map the most important elements in the sample. The x-ray fluorescence tomography is based on the use of the X-ray fluorescence emitted from the elements contained in a sample so as to give additional information to characterize the object under study. In this work a rat lung and two human lung tissue samples have been investigated in order to verify the efficiency of the system in determination of the internal distribution of detected elements in these kinds of samples and to compare the elemental distribution in the lung tissue of an old human and a fetus. The experiments were performed at the X-Ray Fluorescence beamline (XRF) of the Brazilian Synchrotron Light Source (LNLS), Campinas, Brazil. A white beam was used for the excitation of the elements and the fluorescence photons have been detected by a HPGe detector. All the tomographies have been reconstructed using a filtered-back projection algorithm. It was possible to visualize the distribution of high atomic number elements on both, artificial and tissues samples. It was compared the quantity of Zn, Cu and Fe for the lung human tissue samples and verify that these elements have a higher concentration on the fetus tissue sample than the adult tissue sample. (author)

  5. Chemical Characterization of Nuclear Materials: Development a New Combined X-Ray Fluorescence and Raman Spectrometer

    New mobile analytical device based on combination of X-ray fluorescence and Raman spectrometer has been developed for prompt and quantitative characterization of chemical component from Al to U in nuclear waste or undeclared materials. The excitation source of the X-ray fluorescence spectrometer is an air-cooled X-ray tube with Ag transmission anode. For collection of secondary X-ray photons and data processing, a compact Amptek X-ray detector system is applied with silicon drift X-ray detector. The XRF system operates in confocal mode with focal volume around 1-4 mm3. Varying the geometrical position and orientation of the sample optional part of its surface can be analyzed. The Raman unit includes thermoelectrically cooled laser source having 500 mW power at wavelength 785 nm. In order to obtain spectral information from sample surface a reflection-type probe is connected by optical fibres to the Raman spectrometer. A mini focusing optics is set up to the sensor-fibre that provides the system to operate as confocal optical device in reflection mode. The XRF spectrometer with X-ray detector, Raman probe and X-ray tube are mechanically fixed and hermetically connected to an aluminium chamber, which can be optionally filled with helium. The chamber is mounted on a vertical stage that provides moving it to the sample surface. A new model and computer code have been developed for XRF quantitative analysis which describes the mathematical relationship between the concentration of sample elements and their characteristic X-ray intensities. For verification of the calculations standard reference alloy samples were measured. The results was in good agreement with certified concentrations in range of 0.001-100 w%. According to these numerical results this new method is successfully applicable for quick and non-destructive quantitative analysis of waste materials without using standard samples. (author)

  6. X-ray Fluorescence in Member States: Peru. Recent Activities in X ray Fluorescence Laboratory of the Peruvian Institute of Nuclear Energy - Peru

    Multielemental X ray fluorescence non-destructive analysis of the bony remainders attributed to the conqueror Mr. Francisco Pizarro for a study of contamination post-mortem, kind of diet and paleopathologies: The elementary chemical analysis of bones provides very important information that allows studying topics like post mortem contamination, diet and diverse paleopathologies that are observed based on the concentration of the elements identified. The bony remains of the conqueror Don Francisco Pizarro were analyzed by using an energy dispersive X ray fluorescence system with a Cd-109 source of 25 mCi. The spectra were analyzed by IAEA-AXIL-QXAS software. The quantification was carried out with the option of simple quantitative analysis, with the method of elemental sensitivity. The presence of the elements: Ca, Fe, Cu, Zn, Sr and Pb was mainly observed confirming a vegetarian diet and the presence of the surrounding materials. Archaeometric study of metallic pieces from Museo Inka - Universidad Nacional San Antonio Abad from Cusco, Peru: An archaeometric study of metallic pieces, pins (tupus), has been presented. These pieces were found in excavation of Sacsayhuaman strength, Cusco - Peru, from the Inca culture. Metallographic, X ray diffraction and X ray fluorescence analysis of these pieces reveal that pins presents neither the same technology of preparation nor the same elemental composition. All the pieces include copper, as major element, combined with As or Pb. Some of them have a superficial layer of gold and/or silver. Ornamental Nasca ceramics pigments identification by X ray diffraction and X ray fluorescence analysis. The Nasca culture was developed in the southern coast of Peru (100 BC to 650 AD), during the Early Intermediate Period. The most significant remain of the Nasca Culture is the fine polychrome pottery. The goal of this work is to identify the pigments used in 54 pottery fragments recovered nearby Palpa and Cahuachi by using XRF and XRD

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

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

  8. X-ray fluorescence in IAEA Member States: Peru

    The application of the XRF technique performed in our laboratories in the field of archaeology began in 1994. It started with the analysis of different samples, as an incisive tooth, a fragment of occipital, a rib fragment, a segment of dorsal vertebra and small glasses found in the internal surface of a Nazca Culture mummy. In the paleopathological study performed by Dr. Guido Lombardi a 109Cd excitation source and an X ray spectrometry system were used. The elemental concentrations of Ca, Fe, Zn, and Sr were determined for the paleonutricion studies by using the relationships of Zn/Ca and Sr/Ca. The XRF technique also contributed to the mycobacterium tuberculosis detection in a mummy, supplementing other non destructive tests carried out previously. In recent years, 29 right clavicles belonging to mature individuals were analyzed out of 143 found in the Villa El Salvador area. Sr and Zn concentrations were used to determine the relative proportion of vegetable and animal foods in the population's diet under study. It was concluded that the old residents of this town manifested an omnivorous feeding with carnivorous tendency, due to consumption of products of marine origin. Ceramics have also been analyzed to determine the chemical composition of the paste which was used in the production process. 39 fragments of ceramic from the place called Lomo de Corvina of Villa El Salvador, low valley in Lurin town were analyzed. The analysis of these samples was focused on quantitative determination of Ti, Fe, Rb, Sr, Y, Zr and Nb, to complement the results obtained by neutron activation analysis. Identification of the pigments used for production of art objects is of great importance for its characterization, authentication and/or restoration. For this reason, we are currently working on identification of pigments used in the decoration of archaeological ceramics. This work started from construction of a portable XRF spectrometer based on a small size, low power X ray tube

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

    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

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

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

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

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

    2008-09-15

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

  12. An engineering development of fluoroscopic X-ray medical equipment based-on fluorescent screen

    Fluoroscopic x-ray medical equipment uses fluorescent screen to capture structural image of organs. Unlike conventional x-ray equipment which uses film, in the fluoroscopic x-ray, the resulting image is visualized on the fluorescent screen and directly observed by physicians in the patients' rooms. In this study, we developed an image capture system that transforms the image on the fluorescent screen into digital data, which is then transferred to computer for visualization and further processing. By using this system, the observation of the resulting image can be done on a computer that is placed in the control room. The image can also be stored easily and at low cost compared to conventional film. The experiment shows that the system could be used to capture image of the object. However, its quality needs to be improved. In the future, the system will be modified and tested with different types of cameras to obtain better results. (author)

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

    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.

  14. Portable total reflection x-ray fluorescence spectrometer for ultra trace elemental determination

    It has been believed that the use of high power monochromatic incident X-rays such as monochromatic synchrotron radiation is essential for improving detection limits in the total reflection X-ray fluorescence (TXRF) analysis. On the other hand, we have reported that polychromatic excitation improves detection limits in the TXRF analysis compared with monochromatic excitation. We have developed portable TXRF spectrometers using polychromatic X-rays from a low power (several watts) X-ray tube, and a 10 pg (10-11 g) detection limit is achieved with the weak polychromatic X-rays. This low detection limit is obtained using the following methods with polychromatic excitation: (1) measuring smaller amounts of a sample, (2) optimization of a tube voltage, and tube current, (3) optimization of a glancing angle, (4) the use of an appropriate target material of an X-ray tube, and (5) the use of an X-ray waveguide. In the present paper, experimental set-up of the present portable spectrometer and the change of detection sensitivity by changing experimental conditions such as tube voltage are explained. Applications to trace elemental analysis of urine and pigments are also shown. (author)

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

    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.

  16. Development of a total reflection X-ray fluorescence spectrometer for ultra-trace element analysis

    M K Tiwari; B Gowrishankar; V K Raghuvanshi; R V Nandedkar; K J S Sawhney

    2002-10-01

    A simple and fairly inexpensive total reflection X-ray fluorescence (TXRF) spectrometer has been designed, constructed and realized. The spectrometer is capable of ultra-trace multielement analysis as well as performs surface characterization of thin films. The TXRF setup comprises of an X-ray generator, a slitcollimator arrangement, a monochromator/cutoff-stage, a sample reflector stage and an X-ray detection system. The glancing angle of incidence on the two reflectors is implemented using a sine-bar mechanism that enables precise angle adjustments. An energy dispersive detector and a GM counter are employed for measuring respectively the fluorescence intensities and the direct X-ray beam intensity. A Cu-target X-ray generator with its line focus window is used as an excitation source. The spectrometer is quite portable with its compact design and use of a peltier cooled solid state detector for energy dispersive detection. Alignment and characterization of the TXRF system has been performed and the minimum detection limits for various elements have been determined to be in the range of 100 pg to 5 ng even at low X-ray generator powers of 30 kV, 5 mA. The capability of the TXRF system developed for thin film characterization is also demonstrated.

  17. Simultaneous determination of actinides by x-ray fluorescence spectrometry

    The x-ray spectrometric simultaneous determination of uranium and plutonium in simulated Purex Process solutions is described. The method is accomplished by intensity measurements of the L α sub(1) lines. The thin film technique for sample preparation and thorium as an internal standard had been used. An evaporation technique had been also tested for low concentration uranium solutions. In the measurement range 0,05 - 130 U g/L, 0,5 - 20 Pu g/L linear calibration curves were effected. The standard deviation in the concentration range 10 to 130 g/L was 3,5%, 4% in the 1 to 10 g/L and 13% in 0,05 to 1 g/L for uranium determination and 4% for plutonium determination in the range of 1 to 20 g/L. The sensitivity of the method was about 3,62 μg to U and 3,95 μg to Pu. Uranium and plutonium do not reciprocally interfere with one another until U/Pu ≅ 90 m/m. The fission product as interfering elements were also verified. Finally, uranium and plutonium were determined in simulated Purex Process solutions within the requested accuracy for control method. (author)

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

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

    2015-04-21

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

  19. Sc Κα and Κβ X-ray fluorescence spectra

    X-ray fluorescence spectrometry is now one of the most powerful tools for quantitative elemental analysis as well as chemical state analysis of new materials. A complete theoretical understanding of the X-ray emission process still does not exist even after the century following the discovery of X-rays. The major motivation of this study is to clarify the origin of the chemical effects of X-ray emission lines so as to better utilize these chemical effects for chemical state analysis or characterization. The origins of the chemical effects on the XRF satellites of Sc are discussed and a systematic study on the chemical shifts of Sc Kα1 and Kβ1.3 lines of scandium metal and various scandium compounds is presented. (author)

  20. Oscillating dipole model for the X-ray standing wave enhanced fluorescence in periodic multilayers

    André, Jean-Michel; Le Guen, Karine; Jonnard, Philippe

    2013-01-01

    International audience Periodic multilayers give rise to enhanced X-ray fluorescence when a regime of standing waves occurs within the structure. This regime may concern the primary radiation used to induce the fluorescence, the secondary radiation of fluorescence or both of them. Until now, existing models only dealt with standing wave regime of primary radiation. We present a theoretical approach based on the oscillating dipole model and the coupled-wave theory that can treat efficiently...

  1. Langmuir monolayers on water surface investigated by X-ray total reflection fluorescence

    Langmuir monolayers of metal-rich phthalocyanines (Pc) and phospholipid at air/water interface have been studied by X-ray total reflection fluorescence at SR beam line ID 10B (ESRF). Experimental fluorescence angular dependences from 'heavy' ions of a monolayer alone on water surface modulated by evanescent wave/X-ray standing wave pattern have been detected for the first time, are in good agreement with calculations and provide information about the position of metal ions in organic molecule with respect to water surface

  2. Langmuir monolayers on water surface investigated by X-ray total reflection fluorescence

    Zheludeva, S.I.; Novikova, N.N.; Konovalov, O.V.; Kovalchuk, M.V.; Stepina, N.D.; Tereschenko, E.Yu

    2003-10-15

    Langmuir monolayers of metal-rich phthalocyanines (Pc) and phospholipid at air/water interface have been studied by X-ray total reflection fluorescence at SR beam line ID 10B (ESRF). Experimental fluorescence angular dependences from 'heavy' ions of a monolayer alone on water surface modulated by evanescent wave/X-ray standing wave pattern have been detected for the first time, are in good agreement with calculations and provide information about the position of metal ions in organic molecule with respect to water surface.

  3. Influence of crystallinity and polymer matrix on additive quantification by X-ray fluorescence

    Additives are added to polymers during their synthesis, processing or when mixing to other materials and they play an important role on the polymer properties. The objective of this work is to study the influence of the polymer matrix and crystallinity on silicon and other additives quantification by X-ray fluorescence. Initial results showed that X-ray fluorescence can be used to characterize and quantify silicon in polypropylene and in high density polyethylene but it did not show reliable results to linear low density polyethylene and low density polyethylene. (author)

  4. Grazing-emission X-ray fluorescence spectrometry: principles and applications

    Bokx, P.K. de; Kok, C.; Bailleul, A.; Wiener, G.; Urbach, H.P. [Philips Research Labs., Eindhoven (Netherlands)

    1997-06-20

    In grazing emission X-ray fluorescence spectrometry (GEXRF), the sample is irradiated at approximately normal incidence, and only that part of fluorescence radiation is detected that is emitted at grazing angles. This configuration allows the use of wavelength-dispersive detection. This type of detection has the advantages of substantially better energy resolution at longer wavelengths (light elements, L and M lines of heavier elements) and a much larger dynamic range than the energy-dispersive detectors currently used in grazing X-ray techniques. Typical examples are presented of applications that are made possible by this new technique. (Author).

  5. Quantification estimate methods for synchrotron radiation X-ray fluorescence spectroscopy

    Bewer, Brian, E-mail: brian.bewer@lightsource.ca

    2015-03-15

    Synchrotron radiation X-ray fluorescence spectroscopy is a method which allows low elemental concentrations to be measured within a sample. To maintain biological or medical relevance increased importance is being placed on quantifying these in situ localized elemental concentrations. For third generation synchrotron light sources, which have the potential for high sample throughput, a rapid method of obtaining a quantification estimate is needed. Non-destructive transmission and surface analysis techniques for first transition metals, or elements of higher atomic number, using reference standards are examined for different sample property regimes to elucidate methods of quantitative synchrotron radiation X-ray fluorescence spectroscopy.

  6. X-ray fluorescence analysis and optical emission spectrometry of an roman mirror from Tomis, Romania

    The miscellaneous population of Roman Empire, their diverse cultural tradition, their ability to assimilate the roman civilization spirits, had determined a permanent reassessment superimposed upon the roman contribution. Analysis was undertaken using optical emission spectrometry and non-destructive X-ray fluorescence. X-ray fluorescence analysis is a well-established method and is often used in archaeometry and other work dealing with valuable objects pertaining to the history of art and civilization. Roman mirror analysed has been found not to be made of speculum (a high tin bronze). (authors)

  7. X-RAY DIFFRACTION AND X-RAY FLUORESCENCE ANALYSIS OF POTTERY SHARDS FROM NEW ARCHAEOLOGICAL SURVEY IN SOUTH REGION OF SISTAN, IRAN

    Sarhaddi-Dadian, Hossein; Ramli, Zuliskandar; Shuhaimi, Nik Hassan; Rahman, Nik Abdul; Mehrafarin, Reza

    2015-01-01

    The aim of this study is to determine whether pottery shards from new archaeological survey in south region of Sistan are locally made or imported. Many artefacts especially pottery shards have been found during the archaeological survey. These pottery shards are variable in color; from buff, grey, black, and red. The analytical techniques involved X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD), that were applied to determine the major and trace elements and also the mineral content of ...

  8. Development of confocal 3D X-ray fluorescence instrument and its applications to micro depth profiling

    We have developed a confocal micro X-ray fluorescence instrument. Two independent X-ray tubes of Mo and Cr targets were installed to this instrument. Two polycapillary full X-ray lenses were attached to two X-ray tubes, and a polycapillary half X-ray lens was also attached to the X-ray detector (silicon drift detector, SDD). Finally, three focus spots of three lenses were adjusted at a common position. By using this confocal micro X-ray fluorescence instrument, depth profiling for layered samples were performed. It was found that depth resolution depended on energy of X-ray fluorescence that was measured. In addition, X-ray elemental maps were determined at different depths for an agar sample including metal fragments of Cu, Ti and Au. The elemental maps showed actual distributions of metal fragments in the agar, indicating that the confocal micro X-ray fluorescence is a feasible technique for non-destructive depth analysis and 3D X-ray fluorescence analysis. (author)

  9. X-ray fluorescence in IAEA Member States: Croatia

    A beam line attached to the Tandem Van de Graaff accelerator at the Rudjer Boskovic Institute (RBI) in Zagreb, Croatia, has been installed by the IAEA. Seibersdorf. The beam line consists of a vacuum chamber equipped with Si(Li) detector for PIXE spectroscopy positioned at the 135 deg. port, as well as with a particle detector for RBS positioned in the chamber at the 165 degree scattering angle. Recently in 2005, a new 1.0 MV Tandetron accelerator has been installed, enabling use of IAEA beam line with any of two existing accelerators. Homogeneity tests performed by PIXE included tests at microscopic level using RBI nuclear microprobe. Several joint intercomparison tests including two with NIST showed excellent capabilities of the beam line PIXE quantification procedure. Several run sessions were dedicated for PIXE studies a series of archeometry samples of ceramics and polychrome pigments, different geological samples, as well as more recently series of timber species. RBS technique was used for analysis of multilayered thin film technological samples. The use of RBS for the analysis of matrix composition was important for testing reliability of PIXE and XRF quantification procedure based on fundamental parameters. In collaboration with Seibersdorf Laboratories, important improvement has been obtained in development of universal multiparameter data acquisition hardware and software. The software SPECTOR that can control different hardware for data acquisition has, in addition to independent acquisition of spectra from various detectors, the possibility to control sample positioning, as well as microbeam scanning (for proton microbeam at IRB) and sample stage scanning and control (for X ray microbeam at Seibersdorf). Quality control procedures were started to be implemented as well. Operation, measurement and quantification standard operation procedures (SOPs) have been completed

  10. X-ray fluorescence in IAEA Member States: Sri Lanka

    An ED-XRF facility was established in the analytical laboratory of the Atomic Energy Authority of Sri Lanka in 2001 under the technical assistance received through a IAEA TC project. The facility comprises of a X ray tube (Rich - Seifert), a sample holder with secondary target assembly and a Si (Li) detector. The laboratory has also got the necessary facilities to analyze water samples by co-precipitating technique using APDC. Our XRF laboratory has already established analytical procedures to use emission transmission methods (AXIl-QAES, P. Kump), back-scatter fundamental parameter method (QXAS-BFP), APDC co-precipitation method and thin and thick sample analysis method. Selected activities carried out by the XRF Laboratory are: Research study on heavy metal concentration levels in crow feathers collected from different environments and in industrial effluents released to a main water body (i.e the Kelani River); Research study on hyper accumulating capacity of flora in Ussangoda area (Serpentine mineral deposited area); Study on the possibility of removing heavy metals in liquid waste by bricks (low cost waste water treatment method); Study on heavy metal contamination in soil collected from Tsunami affected areas; Elemental analysis of air particulate matter to identify pollutants and pollution sources; Provision of analytical services to archaeological studies; Alloy analysis for technical evaluations. In Sri Lanka, there is a rising demand for this analytical service as it can provide the customer relatively fast and reliable results at low cost. AEA has decided to upgrade the existing facility to TXRF through the IAEA technical assistance to meet the demand for the services to analyse water and other liquid samples. In addition, Quality Assurance and Quality control procedures have been implemented for validation of analytical methods and check of accuracy of analytical results obtained

  11. Application of x-ray fluorescence to the measurement of additives in paper

    Titanium dioxide content in paper was measured by x-ray fluorescence analysis using an 55Fe source and an x-ray proportional counter to determine the feasibility of an on-line instrument. X-ray calibration curves for 60- and 100-g/m2 paper samples were obtained using neutron activation to measure the titanium dioxide concentration. The predictions of a simple model were in good agreement with the experimental calibration curves. The measurements and calculations were extended to investigate the effects of clay and moisture. The presence of clay has a significant effect on the x-ray fluorescence determination of the titanium dioxide concentration; however, this can be well accounted for by the model. The calculations indicated that the effect of typical moisture levels on the titanium dioxide determination was small and can be ignored. It is not possible to measure the clay content by x-ray fluorescence; however, preliminary results for the determination of calcium carbonate concentration are promising

  12. Influence of X-ray tube spectral distribution on uncertainty of calculated fluorescent radiation intensity

    The relative radiation intensity (Ri) defined as fluorescent radiation intensity of analyte in specimen to fluorescent radiation intensity of pure element or compound, e.g., oxide is used in calculation in both fundamental parameter methods and in theoretical influence coefficient algorithms. Accuracy of calculated Ri is determined by uncertainties of atomic parameters, spectrometer geometry and also by X-ray tube spectral distribution. This paper presents the differences between Ri calculated using experimental and theoretical X-ray tube spectra evaluated by three different algorithms proposed by Pella et al., Ebel, and Finkelshtein-Pavlova. The calculations are performed for the most common targets, i.e., Cr, Mo, Rh and W. In this study, Ri is calculated for V, Cr, Mn, Fe, Co, Ni, Cu and Mo in steels as an example. The differences between Ri calculated using different X-ray tube spectrum algorithms are presented when pure element standard, multielement standard similar to the analyzed material and one pure element standard for all analytes is used in X-ray fluorescence analysis. The differences between Ri for intermediate-thickness samples (and also for thin films) and for X-ray tube, which ran for many hours, are also evaluated

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

    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}.

  14. Sediment U, Th, K content analyzed using X-ray fluorescence spectrometry for ESR dating samples

    The accurate measurement of dose rate is the key issues to obtain reliable ESR age. In this article, we used X-ray fluorescence spectrometry to determine the U, Th, K content of the fluvial sediments. And the standard working curves were established using the national rock reference material. Setting the lower X-ray power and the matrix effect, U, Th, K content in the fluvial sediment were investigated. The results show that the method recovery rate of U and Th is less than 15%. Comparing with the measurement data from the α-counting and Atomic Spectrometry analysis, the dose rate difference is less than 5%. It shows that the X-ray fluorescence spectrometry method can fit for the requirement for obtaining the U, Th, K content of fluvial sediment for ESR dating. (authors)

  15. Optimizing the flotation technologies by means of on-stream X-ray fluorescence analysis

    X-ray fluorescence analysis has been successfully applied for more than 20 years in different instrumental configuration for the purpose of optimizing and controlling the ore processing technological processes performed by flotation. The paper presents a recent achievement provided with an on-stream X-ray fluorescence analytical system implemented at the Baia Mare Flotation Center within a cooperation project between ICPM Baia Mare and the 'Tvetmetavtomatika' Institute in Moscow - Russia. The paper includes the construction of the system, the operating characteristics of the 'SRM-13' type X-ray spectrometers, the mathematical model used for their calibration for analyzing the pulp samples, required sensitivity corrections and accuracy and the resulting technical-economical effects as well. (Author)

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

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

  17. Three dimensional subsurface elemental identification of minerals using confocal micro-X-ray fluorescence and micro-X-ray computed tomography

    Current non-destructive elemental characterization methods, such as scanning electron microscopy-based energy dispersive spectroscopy (SEM–EDS) and micro-X-ray fluorescence spectroscopy (MXRF), are limited to either elemental identification at the surface (SEM–EDS) or suffer from an inability to discriminate between surface or depth information (MXRF). Thus, a non-destructive elemental characterization of individual embedded particles beneath the surface is impossible with either of these techniques. This limitation can be overcome by using laboratory-based 3D confocal micro-X-ray fluorescence spectroscopy (confocal MXRF). This technique utilizes focusing optics on the X-ray source and detector which allows for spatial discrimination in all three dimensions. However, the voxel-by-voxel serial acquisition of a 3D elemental scan can be very time-intensive (~ 1 to 4 weeks) if it is necessary to locate individual embedded particles of interest. As an example, if each point takes a 5 s measurement time, a small volume of 50 × 50 × 50 pixels leads to an acquisition time of approximately 174 h, not including sample stage movement time. Initially screening the samples for particles of interest using micro-X-ray computed tomography (micro-CT) can significantly reduce the time required to spatially locate these particles. Once located, these individual particles can be elementally characterized with confocal MXRF. Herein, we report the elemental identification of high atomic number surface and subsurface particles embedded in a mineralogical matrix by coupling micro-CT and confocal MXRF. Synergistically, these two X-ray based techniques first rapidly locate and then elementally identify individual subsurface particles. - Highlights: • Coupling of confocal X-ray fluorescence spectroscopy and X-ray computed tomography • Qualitative elemental identification of surface and subsurface mineral particles • Non-destructive particle size measurements • Utilization of

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

    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

  19. Ray-tracing of a Real-Time X-Ray Fluorescence Microscope

    The author is doing the conceptual design of the Real-time X-ray Fluorescence Microscope (R-XRFM) which can perform elemental mapping by X-ray fluorescence without scanning the sample. Doubly curved crystal of a Johansson type monochromator or a Johann type monochromator will be used as a point-to-point focus monochromator in R-XRFM and the performances in each case were evaluated by simulation calculation using ray-tracing method. From the result of the calculation in conditions of a 60 mm diameter α-quartz crystal monochromator, a 300 mm radius Rowland circle, and an X-ray fluorescence wavelength of Al Kα1, in both cases of the Johansson type and in case of the Johann type 40 mm in width, it was found that the angular resolution is 0.010deg, and there is a possibility that R-XRFM can perform elemental mapping identifying the differences in the fluorescent X-ray wavelength of the aluminum due to the difference in the coordination number. In the case of Johansson type, it was found that the X-rays converge on the detector surface with the spatial resolution < 0.001-1.3 μm from the analyzing area of 0-50 μm square, and with the spatial resolution 1.3-2.5 μm from the analyzing area of 50-100 μm square. In the case of Johann type 40 mm in width, it was found that the X-rays converge on a detector surface with the spatial resolution 1.5-3.7 μm from the analyzing area of 0-100 μm square. (author)

  20. Mobile low power total reflexion x-ray fluorescence spectrometer with pg-detection-limit

    Full text: Total reflexion x-ray fluorescence (TXRF) spectrometry is an efficient tool in trace element analysis. Conventional laboratory spectrometers can achieve detection limits in the pg-range. Unfortunately high power X-ray tubes (i.e. some kW) and LN2-cooled Si(Li)-detectors are sometimes not applicable within mobile TXRF-spectrometers. Therefore a portable device for TXRF (PicoTAXPS) has been developed and the latest results will be presented. This device is a very compact combination of an air-cooled low power X-ray tube (Mo-anode, 40W) a Peltier-cooled PlN-diode detector and a high quality flat primary Ni/C X-ray mirror (2t= 7.84 nm, N100, R> 80%). The background radiation is reduced by means of this particular mirror. That way the achievable detection limits are comparable with conventional 1.5 kW TXRF- spectrometers. The characteristic parameters of X-ray source, detector and Ni/C mirror will be presented. Additionally, the performance of this portable TXRF-system will be demonstrated by selected examples. Copyright (1999) Australian X-ray Analytical Association Inc

  1. Formation of binary and ternary metal deposits on glass-ceramic carbon electrode surfaces: electron-probe X-ray microanalysis, total-reflection X-ray fluorescence analysis, X-ray photoelectron spectroscopy and scanning electron microscopy study

    The features of the formation of binary and ternary alloys during the electrochemical deposition and co-deposition of copper, cadmium and lead from aqueous solutions on disc glass-ceramic carbon electrode surfaces were studied by electron-probe X-ray microanalysis, total-reflection X-ray fluorescence analysis, X-ray photoelectron spectroscopy and scanning electron microscopy. The macroscopic properties of electrodeposits such as morphology, lateral distribution of the elements along the disc electrode surface and depth distribution of the elements in the electrodeposit bulk were established. The mechanisms of metal nucleation and growth of thin films of electrodeposits were discussed

  2. X-ray fluorescence method in analyzing forest fire emission elements

    Composition of aerosols from large taiga forest fires was investigated using an X-ray fluorescence method that involves excitation of the characteristic spectrum by synchrotron radiation. Emissions were sampled directly from the convection column with the help of various instruments (including an impactor) mounted on a helicopter. We compared the results of the study with literature data

  3. Fast, versatile x-ray fluorescence method for measuring tin in impregnated wood

    Drabæk, I.; Christensen, Leif Højslet

    1985-01-01

    The present paper describes an energy-dispersive x-ray fluorescence method for measuring tin in bis(tri-n-butyl)tin-oxide impregnated wood. The proposed method is of the backscatter/fundamental parameter type. Its versatility, precision, and accuracy is demonstrated by analyses of eleven samples of...

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

    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.

  5. Trace element analysis of red beet and its cell cultures by x-ray fluorescence method

    Cell cultures from red beet root and beet sprout were analysed by isotope excited energy-dispersive X-ray fluorescence method. The excitation source was 125I. High zinc ion concentrations were found in cell cultures together with high histidine content. (author)

  6. Some applications of x-ray fluorescence spectrography to the determination of uranium and thorium

    Several methods for the determination of uranium and thorium by X-ray fluorescence spectrography are described. In pure solutions the sensitivity for these elements is 5-10 ppm. For solutions containing gross concentrations of impurities, strontium is added as an internal standard. Precision and accuracy of the determinations are about 1% when working in the optimum concentration range. (author)

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

    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.…

  8. Certification of reference materials by energy-dispersive x-ray fluorescence spectrometry

    The present paper studies the precision and accuracy that can be achieved using energy-dispersive x-ray fluorescence spectrometry for the determination of total sulphur content in BCR 38 Fly Ash issued by the European Community Bureau of Reference

  9. Confirmation of molecular formulas of metallic complexes through X-ray fluorescence quantitative analysis

    X-ray fluorescence spectrophotometry was employed to determined the metal content in a series of five transition element complexes (Mn, Ti, Zn, V). The results confirmed the molecular formulas of these complexes, already proposed on the basis of elemental microanalysis, solution condutimetry and other analytical methods. (C.L.B.)

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

    Hiller, L

    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.

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

    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.

  12. Preliminary experiment of fluorescent X-ray computed tomography to detect dual agents for biological study.

    Yu, Q; Takeda, T; Yuasa, T; Hasegawa, Y; Wu, J; Thet-Thet-Lwin; Hyodo, K; Dilmanian, F A; Itai, Y; Akatsuka, T

    2001-05-01

    The simultaneous observation of various information, such as blood flow, tissue metabolism and distribution of receptors, is quite important in order to understand the functional state of biomedical objects. The simultaneous detectability of contrast agents by fluorescent X-ray computed tomography (FXCT) with synchrotron radiation is examined in this study. The system consisted of a silicon (111) double-crystal monochromator, an X-ray slit system, a scanning table, a PIN diode, a highly purified germanium detector and an X-ray charge-coupled device (CCD) camera. The monochromatic X-ray beam energy was adjusted to 37.0 keV and collimated into a pencil beam of 1 x 1 mm. The fluorescent spectra of the K alpha lines for iodine and xenon were detected simultaneously. FXCT could image the distribution of both iodine and xenon agents in a phantom clearly and the contrast ratio was significantly better than that of transmission X-ray computed tomography images. PMID:11486409

  13. X-ray Fluorescence in Member States: Spain. Activities at the Laboratory of X ray Analytical Applications (LARX)

    1. Determination of Metal Residues in Active Pharmaceutical Ingredients According to Current Legislation by Using XRF Spectrometry. Safety and efficacy of pharmaceuticals are two fundamental issues of importance in drug therapy. Therefore, the determination of potential impurities in different stages of the manufacturing processes, and especially in the final product, is necessary to prevent potential risk to human health. Metals can be introduced in the active pharmaceutical ingredients (API) through different sources (raw materials, reagents, catalysts, reactors, etc) and, consequently, they are potential impurities in the drug substances and are routinely monitored. 2. Application of XRF Spectrometry in Phytoremediation Activities Around Mining Areas. In the last decade, the use of plants for the stabilization (phytostabilization) and clean-up (phytoremediation) of metal contaminated environments has gained popularity among government agencies worldwide, as alternate or complementary cost-effective non-invasive technology to the engineering based remediation methods. In view of the considerable number of analyses necessary in phytoremediation and plant biology studies, it is important that the analytical procedures used for elemental determination in plant tissues should be fast and cheap, with simple sample preparation, and of adequate accuracy and precision. Last years, we have developed several analytical methodologies, using diverse configurations of XRF spectrometers (EDXRF, WDXRF, HE-P-EDXRF), to determine elemental composition of vegetation grown in mining areas. Recently, in collaboration with a research group from the Department of Chemical Engineering, Agriculture and Food Technology of the University of Girona (Spain), we have studied the possibilities and limitations of a low-cost benchtop energy dispersive X ray fluorescence (EDXRF) instrument to be employed as analytical technique for studying the potential use of sunflowers (Helianthus annuus) for

  14. Influence of angle's ranges for recording an X-ray fluorescence hologram on reconstructed atomic images

    XIE Hong-Lan; CHEN Jian-Wen; GAO Hong-Yi; ZHU Hua-Feng; LI Ru-Xin; XU Zhi-Zhan

    2004-01-01

    X-ray fluorescence holography (XFH) is a novel method for three-dimensional (3D) imaging of atomic structure. Theoretically, in an XFH experiment, one has to measure the fluorescence energy on a spherical surface to get well-resolved 3D images of atoms. But in practice, the experimental system arrangement does not allow the measurement of the fluorescent intensity oscillations in the full sphere. The holographic information losses because of the limited sampling range (less than 4π) will directly result in defective reconstructed atomic images. In this work, the atomic image of a Fe single crystal (001) was reconstructed by numerically simulating X-ray fluorescence holograms of the crystal at different recording angle's ranges and step lengths. Influences of the ranges of azimuth angles and polar angles and the step length of polar angles on the reconstructed atomic images were discussed.

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

    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 Kα and Kβ 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

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

    Wang, Xin [Univ. of California, Davis, CA (United States). Dept. of Applied Science

    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.

  17. Improving x-ray fluorescence signal for benchtop polychromatic cone-beam x-ray fluorescence computed tomography by incident x-ray spectrum optimization: A Monte Carlo study

    Manohar, Nivedh [Nuclear/Radiological Engineering and Medical Physics Programs, Woodruff School of Mechanical Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332 (United States); Jones, Bernard L. [Department of Radiation Oncology, University of Colorado School of Medicine, Aurora, Colorado 80045 (United States); Cho, Sang Hyun, E-mail: scho@mdanderson.org [Department of Radiation Physics and Department of Imaging Physics, The University of Texas MD Anderson Cancer Center, Houston, Texas 77030 (United States)

    2014-10-15

    Purpose: To develop an accurate and comprehensive Monte Carlo (MC) model of an experimental benchtop polychromatic cone-beam x-ray fluorescence computed tomography (XFCT) setup and apply this MC model to optimize incident x-ray spectrum for improving production/detection of x-ray fluorescence photons from gold nanoparticles (GNPs). Methods: A detailed MC model, based on an experimental XFCT system, was created using the Monte Carlo N-Particle (MCNP) transport code. The model was validated by comparing MC results including x-ray fluorescence (XRF) and scatter photon spectra with measured data obtained under identical conditions using 105 kVp cone-beam x-rays filtered by either 1 mm of lead (Pb) or 0.9 mm of tin (Sn). After validation, the model was used to investigate the effects of additional filtration of the incident beam with Pb and Sn. Supplementary incident x-ray spectra, representing heavier filtration (Pb: 2 and 3 mm; Sn: 1, 2, and 3 mm) were computationally generated and used with the model to obtain XRF/scatter spectra. Quasimonochromatic incident x-ray spectra (81, 85, 90, 95, and 100 keV with 10 keV full width at half maximum) were also investigated to determine the ideal energy for distinguishing gold XRF signal from the scatter background. Fluorescence signal-to-dose ratio (FSDR) and fluorescence-normalized scan time (FNST) were used as metrics to assess results. Results: Calculated XRF/scatter spectra for 1-mm Pb and 0.9-mm Sn filters matched (r ≥ 0.996) experimental measurements. Calculated spectra representing additional filtration for both filter materials showed that the spectral hardening improved the FSDR at the expense of requiring a much longer FNST. In general, using Sn instead of Pb, at a given filter thickness, allowed an increase of up to 20% in FSDR, more prominent gold XRF peaks, and up to an order of magnitude decrease in FNST. Simulations using quasimonochromatic spectra suggested that increasing source x-ray energy, in the

  18. Improving x-ray fluorescence signal for benchtop polychromatic cone-beam x-ray fluorescence computed tomography by incident x-ray spectrum optimization: A Monte Carlo study

    Purpose: To develop an accurate and comprehensive Monte Carlo (MC) model of an experimental benchtop polychromatic cone-beam x-ray fluorescence computed tomography (XFCT) setup and apply this MC model to optimize incident x-ray spectrum for improving production/detection of x-ray fluorescence photons from gold nanoparticles (GNPs). Methods: A detailed MC model, based on an experimental XFCT system, was created using the Monte Carlo N-Particle (MCNP) transport code. The model was validated by comparing MC results including x-ray fluorescence (XRF) and scatter photon spectra with measured data obtained under identical conditions using 105 kVp cone-beam x-rays filtered by either 1 mm of lead (Pb) or 0.9 mm of tin (Sn). After validation, the model was used to investigate the effects of additional filtration of the incident beam with Pb and Sn. Supplementary incident x-ray spectra, representing heavier filtration (Pb: 2 and 3 mm; Sn: 1, 2, and 3 mm) were computationally generated and used with the model to obtain XRF/scatter spectra. Quasimonochromatic incident x-ray spectra (81, 85, 90, 95, and 100 keV with 10 keV full width at half maximum) were also investigated to determine the ideal energy for distinguishing gold XRF signal from the scatter background. Fluorescence signal-to-dose ratio (FSDR) and fluorescence-normalized scan time (FNST) were used as metrics to assess results. Results: Calculated XRF/scatter spectra for 1-mm Pb and 0.9-mm Sn filters matched (r ≥ 0.996) experimental measurements. Calculated spectra representing additional filtration for both filter materials showed that the spectral hardening improved the FSDR at the expense of requiring a much longer FNST. In general, using Sn instead of Pb, at a given filter thickness, allowed an increase of up to 20% in FSDR, more prominent gold XRF peaks, and up to an order of magnitude decrease in FNST. Simulations using quasimonochromatic spectra suggested that increasing source x-ray energy, in the

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

    Sun, Yue, E-mail: ysun@u.northwestern.edu [Graduate Program in Applied Physics, Northwestern University, Evanston, IL 60208 (United States); Gleber, Sophie-Charlotte, E-mail: gleber@aps.anl.gov [Argonne National Laboratory, Argonne, IL 60439 (United States); Jacobsen, Chris, E-mail: cjacobsen@anl.gov [Argonne National Laboratory, Argonne, IL 60439 (United States); Department of Physics and Astronomy, Northwestern University, Evanston, IL 60208 (United States); Chemistry of Life Processes Institute, Northwestern University, Evanston, IL 60208 (United States); Kirz, Janos, E-mail: jkirz@lbl.gov [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Vogt, Stefan, E-mail: vogt@aps.anl.gov [Argonne National Laboratory, Argonne, IL 60439 (United States)

    2015-05-15

    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. - Highlights: • We present a model for x-ray fluorescence detection with scanned x-ray beams. • We use it to compare detector

  20. X-Ray Fluorescence Spectrometry. II. Determination of Uranium in ores

    A method of analysis of uranium in ores by X-ray spectrometry was developed, using the internal standard technique. Strontium was found to be the most suitable internal standard for general use. A Norelco Philips X-ray fluorescent spectrometer was used in this work, equipped with a lithium fluoride crystal acting as a diffraction grating analyzer. The intensity of the uranium-L α1 spectral line is calculated and related to corresponding strontium-Kα spectral line, both detected with a Scintillation Counter. (Author) 31 refs

  1. Chlorophyll Fluorescence Spectra as an Indicator of X-Ray + EMS-Induced Phytotoxicity in Safflower

    Pandey, Jitendra Kumar; Srivastava, Preeti; Yadav, Ram Singh; Gopal, Ram

    2012-01-01

    The present investigation deals with the study of in vivo laser-induced chlorophyll florescence spectra (LICF) of safflower leaves (Carthamus tinctorius L.) for X-rays + EMS-treated plants. Seeds were treated with different doses of X-ray + EMS (5, 8, 12, 25, and 30 Kr + 0.5% EMS) and were grown in the green house. The effects of the concerned treatment on chlorophyll (Chl) contents and Chl fluorescence were investigated after 7 days of germination. Results obtained revealed that the values o...

  2. Analysis of siliceous geologic materials by energy-dispersive X-ray fluorescence

    The determination of the elements Al, Si, K, Ca, Ti, Cr, Mn and Fe in siliceous geologic samples by energy-dispersive X-ray fluorescence is investigated using the most adequate excitation conditions: direct excitation mode (rhodium anode X-ray tube) for the former two elements, and the secondary targets titanium for K and Ca, and germanium for Ti, Cr, Mn and Fe. For the correction of matrix effects the use of ratio methods has been tested. Procedure files have been defined allowing the automatic simultaneous acquisition and processing of spectra. (author)

  3. Determination of Co in MgO matrix by wavelength dispersive X-ray fluorescence technique

    A Wavelength Dispersive X-ray Fluorescence (WDXRF) method for the analysis of Co in Mg matrix has been developed. The minimum determination limit achieved is 1 ppm. Special care has been taken in making the double layer pellet of synthetic standards such that the pellet after several exposures to x-rays does not become brittle. The working range for this method is 1-100 ppm. The relative percentage standard deviation calculated for the above range varies from 21% to 0.5%. (author)

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

    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. - Highlights: • We present a model for x-ray fluorescence detection with scanned x-ray beams. • We use it to compare detector

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

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

    2016-04-01

    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.

  6. Comparing the Ag-content of poltinniks using X-ray fluorescence

    Ferguson, S

    2013-01-01

    X-ray fluorescence experiments have been performed in order to analyze the elemental composition of four Russian 50-kopek coins ("poltinniks") minted during 1913, 1921, and 1924. By comparing the intensities of the Ag K{\\alpha} X-rays emitted by the poltinniks, we were able to determine whether the Ag-content of the coins were equal. One of the goals of this study was to determine whether or not legislation was carried out that required the proportions of Ag and Cu used in the minting of coins in 1924 to be identical to those minted in previous years. Also, the intensities of the Ag K{\\alpha} X-rays emitted by 1924 poltinniks minted in London and Leningrad were compared. Our results suggest that the percent difference in the proportions of Ag present in each of the coins is no more than 5.5%.

  7. Gold estimation in geological samples using energy dispersive X-ray fluorescence spectroscopy

    Gold concentration in Indus river sediments have been estimated using energy dispersive X-ray fluorescence (EDXRF) spectrometry. To get the best possible detection sensitivity, optimisation of sample preparation procedure and exciting radiation was done. Physical preconcentration procedure of panning of heavy minerals has been employed. Samples were dissolved in acqua regia to homogenize the distribution of gold. For obtaining an optimum excitation sensitivity, radioisotope sources of various energies as well as a low power laboratory built transmission type Mo X-ray tube have been used. L shell X-rays of gold have been used for qualitative analysis. For quantitative estimation, a combination of single element fundamental parameter method and scattered radiation standardisation method was used. The sensitivity of EXDRF spectrometer for gold was around 50 ppm. (author). 6 figs., 2 tables

  8. Dosage of silicon in a soluble silicate using an x-ray-fluorescence radioisotopic method

    A description is given of a spectrometer for X ray fluorescence analysis having a radio active excitation source. It has been applied to the analysis of the silicon contained in an industrial soluble silicate. A theoretical study has been made for this analysis of the operational conditions such as: the effect of the particle size, the dilution of the sample, the sensitivity as a function of the X ray excitation energy. It is possible to obtain a relative accuracy of 0,87 per cent for the silicon determination, for one standard deviation. A comparison is made of the sensitivity obtained using this apparatus for the Si determination with that which can be obtained using a conventional apparatus fitted with an X ray tube. (author)

  9. Application of X-ray fluorescence analytical techniques in phytoremediation and plant biology studies

    Necemer, Marijan [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia)], E-mail: marijan.necemer@ijs.si; Kump, Peter; Scancar, Janez; Jacimovic, Radojko; Simcic, Jurij; Pelicon, Primoz; Budnar, Milos; Jeran, Zvonka [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia); Pongrac, Paula; Regvar, Marjana; Vogel-Mikus, Katarina [Department of Biology, Biotechnical Faculty, University of Ljubljana, Vecna pot 111, SI-1000 Ljubljana (Slovenia)

    2008-11-15

    Phytoremediation is an emerging technology that employs the use of higher plants for the clean-up of contaminated environments. Progress in the field is however handicapped by limited knowledge of the biological processes involved in plant metal uptake, translocation, tolerance and plant-microbe-soil interactions; therefore a better understanding of the basic biological mechanisms involved in plant/microbe/soil/contaminant interactions would allow further optimization of phytoremediation technologies. In view of the needs of global environmental protection, it is important that in phytoremediation and plant biology studies the analytical procedures for elemental determination in plant tissues and soil should be fast and cheap, with simple sample preparation, and of adequate accuracy and reproducibility. The aim of this study was therefore to present the main characteristics, sample preparation protocols and applications of X-ray fluorescence-based analytical techniques (energy dispersive X-ray fluorescence spectrometry-EDXRF, total reflection X-ray fluorescence spectrometry-TXRF and micro-proton induced X-ray emission-micro-PIXE). Element concentrations in plant leaves from metal polluted and non-polluted sites, as well as standard reference materials, were analyzed by the mentioned techniques, and additionally by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). The results were compared and critically evaluated in order to assess the performance and capability of X-ray fluorescence-based techniques in phytoremediation and plant biology studies. It is the EDXRF, which is recommended as suitable to be used in the analyses of a large number of samples, because it is multi-elemental, requires only simple preparation of sample material, and it is analytically comparable to the most frequently used instrumental chemical techniques. The TXRF is compatible to FAAS in sample preparation, but relative to AAS it is fast, sensitive and

  10. Application of X-ray fluorescence analytical techniques in phytoremediation and plant biology studies

    Phytoremediation is an emerging technology that employs the use of higher plants for the clean-up of contaminated environments. Progress in the field is however handicapped by limited knowledge of the biological processes involved in plant metal uptake, translocation, tolerance and plant-microbe-soil interactions; therefore a better understanding of the basic biological mechanisms involved in plant/microbe/soil/contaminant interactions would allow further optimization of phytoremediation technologies. In view of the needs of global environmental protection, it is important that in phytoremediation and plant biology studies the analytical procedures for elemental determination in plant tissues and soil should be fast and cheap, with simple sample preparation, and of adequate accuracy and reproducibility. The aim of this study was therefore to present the main characteristics, sample preparation protocols and applications of X-ray fluorescence-based analytical techniques (energy dispersive X-ray fluorescence spectrometry-EDXRF, total reflection X-ray fluorescence spectrometry-TXRF and micro-proton induced X-ray emission-micro-PIXE). Element concentrations in plant leaves from metal polluted and non-polluted sites, as well as standard reference materials, were analyzed by the mentioned techniques, and additionally by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). The results were compared and critically evaluated in order to assess the performance and capability of X-ray fluorescence-based techniques in phytoremediation and plant biology studies. It is the EDXRF, which is recommended as suitable to be used in the analyses of a large number of samples, because it is multi-elemental, requires only simple preparation of sample material, and it is analytically comparable to the most frequently used instrumental chemical techniques. The TXRF is compatible to FAAS in sample preparation, but relative to AAS it is fast, sensitive and

  11. Application of X-ray fluorescence analytical techniques in phytoremediation and plant biology studies

    Nečemer, Marijan; Kump, Peter; Ščančar, Janez; Jaćimović, Radojko; Simčič, Jurij; Pelicon, Primož; Budnar, Miloš; Jeran, Zvonka; Pongrac, Paula; Regvar, Marjana; Vogel-Mikuš, Katarina

    2008-11-01

    Phytoremediation is an emerging technology that employs the use of higher plants for the clean-up of contaminated environments. Progress in the field is however handicapped by limited knowledge of the biological processes involved in plant metal uptake, translocation, tolerance and plant-microbe-soil interactions; therefore a better understanding of the basic biological mechanisms involved in plant/microbe/soil/contaminant interactions would allow further optimization of phytoremediation technologies. In view of the needs of global environmental protection, it is important that in phytoremediation and plant biology studies the analytical procedures for elemental determination in plant tissues and soil should be fast and cheap, with simple sample preparation, and of adequate accuracy and reproducibility. The aim of this study was therefore to present the main characteristics, sample preparation protocols and applications of X-ray fluorescence-based analytical techniques (energy dispersive X-ray fluorescence spectrometry—EDXRF, total reflection X-ray fluorescence spectrometry—TXRF and micro-proton induced X-ray emission—micro-PIXE). Element concentrations in plant leaves from metal polluted and non-polluted sites, as well as standard reference materials, were analyzed by the mentioned techniques, and additionally by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). The results were compared and critically evaluated in order to assess the performance and capability of X-ray fluorescence-based techniques in phytoremediation and plant biology studies. It is the EDXRF, which is recommended as suitable to be used in the analyses of a large number of samples, because it is multi-elemental, requires only simple preparation of sample material, and it is analytically comparable to the most frequently used instrumental chemical techniques. The TXRF is compatible to FAAS in sample preparation, but relative to AAS it is fast

  12. Application of X ray fluorescence techniques for the determination of hazardous and essential trace elements in environmental and biological materials

    Full text: The utilization of X ray fluorescence (XRF) technique for the determination of trace element concentrations in environmental and biological samples is presented. The analytical methods used include energy dispersive X ray fluorescence (EDXRF), total reflection X ray fluorescence (TXRF), micro-beam X ray fluorescence and direct in situ X-ray fluorescence analysis. The measurements have been performed with X ray tube- and radioisotope-based energy dispersive X ray fluorescence spectrometers. Both liquid nitrogen- and thermo electrically-cooled silicon detectors were utilized in the analysis. Samples analysed include soil, water, plant material, and airborne particulate matter collected on filters. Depending on the technique and the investigated elements, the above-mentioned samples were analysed either directly or indirectly (after decomposing the sample in a mineralization process or/and chemical preconcentration procedure). The achieved detection limits for different techniques, established by measuring appropriate reference standards, are presented. The utilization of the micro-beam XRF technique for studying element distribution in heterogeneous samples and investigating the 3D- and 2D-morphology of minute samples by means of computerized X ray absorption and X ray fluorescence tomography is described. The different X ray techniques have their unique advantages. The micro-beam X ray fluorescence set-up has an advantage of producing very well collimated primary X ray beam (by means of X ray capillary optics the beam is collimated down to about 15 μm in diameter), in front of which the analysed sample can be precisely positioned, providing local information about the sample composition. TXRF technique has its leading edge in analysis of liquid samples, and as a reference method for a conventional bulk EDXRF analysis of heterogeneous materials such as air particulates collected on filter where the particle size effects can seriously influence the

  13. An imaging X-ray fluorescence spectrometer for near earth objects

    We propose a novel imaging X-ray spectrometer to be flown on a space mission to a Near Earth Object (NEO) (the Moon, a near Earth asteroid or a comet). In either of the first two cases the instrument will record X-ray fluorescence excited from the surface by the solar X-ray flux to form 'compositional maps' of its surface, providing valuable information on the evolution of these objects. In the case of a comet, the device will study the X-ray emission resulting from its interaction with the solar wind. During cruise when the spacecraft is en-route to the NEO the instrument will be used to make astronomical observations of Active Galactic Nuclei (AGN), X-ray binary stars and coronal sources in star clusters such as the Pleiades or Hyades. The instrument, proposed for ESA's SMART-1 mission, is a miniature telescope, of 37.5 cm focal length, based on microchannel plate (MCP) optics and charged coupled device (CCD) detectors providing both imaging and a medium resolution ∼50-100 eV spectroscopic capability; sufficient to resolve the L lines of Ca, Ti, Fe, and the K lines of O, Mg, Al and Si with an angular resolution ∼10 arcmin and a 6x6 deg. field of view

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

    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. PMID:25025342

  15. X-ray fluorescence applied to the fission time study of Z=120 element

    Characteristic X-rays of the element Z=120 have been identified in the reaction 238U+64Ni at 6,6 MeV per nucleon. They have been detected in coincidence with fission fragments arising from composite systems with 120 protons formed during the reaction. Pieces of information about the formation probability by fusion of Z=120 nuclei and on the fission time of this nucleus have been inferred from the X-ray multiplicity. From the maximal measured X-ray multiplicity and with the assumption of an exponential distribution of fission times, we have determined an inferior limit of 4.0*10-18 s for the mean fission time of Z=120 nuclei. This maximal measured X-ray has also allowed us to state that at best 38% of capture reactions (it means quasi-fission + fusion reactions) correspond to quasi-fission reactions associated with times below than 10-19 seconds. This relatively low percentage of quasi-fission reactions is not consistent with the very low fusion probabilities generally expected for our system. This work has shown that the X-ray fluorescence technique can be used successfully for studying the stability of super-heavy elements

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

    Carlisle, J.A.; Chaiken, A.; Michel, R.P. [Lawrence Berkeley National Lab., CA (United States)] [and others

    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.

  17. Utilization of fluorescent uranium x-rays as verification tool for irradiated CANDU fuel bundles

    The use of fluorescent uranium x-rays for in-situ safeguards verification of irradiated CANDU fuel bundles is described. Room temperature CdZnTe (supergrade) semiconductor detector of low sensitivity coupled to charge sensitive pre-amplifier is used. This detector is characterized by moderate resolving power in the low energy region around 100 keV. It as such allows the separation of uranium x-rays in the close proximity of tungsten x-rays emanating from the shielding/collimator assembly. On account of strong attenuation, the detection of low energy x-rays requires the shielding to be of an optimized thickness. Further, in view of high intensity of this radiation the use of small volume detector is warranted. In dealing with the subject, this paper therefore presents an assessment, not only of the detector but also the shield-collimator assembly for the required verification of short cooling time fuel bundles. Results of the associated optimization measurements with respect to collimator aperture and detector sensitivity are consequently included. The future course of work from the viewpoint of development of a suitable x-ray spectrometer specifically for the purpose of verifying extremely short (< 1 month old) cooling time fuel bundles is moreover identified. (author)

  18. A flexible setup for angle-resolved X-ray fluorescence spectrometry with laboratory sources

    Spanier, M.; Herzog, C.; Grötzsch, D.; Kramer, F.; Mantouvalou, I.; Lubeck, J.; Weser, J.; Streeck, C.; Malzer, W.; Beckhoff, B.; Kanngießer, B.

    2016-03-01

    X-ray fluorescence (XRF) analysis is one of the standard tools for the analysis of stratified materials and is widely applied for the investigation of electronics and coatings. The composition and thickness of the layers can be determined quantitatively and non-destructively. Recent work showed that these capabilities can be extended towards retrieving stratigraphic information like concentration depth profiles using angle-resolved XRF (ARXRF). This paper introduces an experimental sample chamber which was developed as a multi-purpose tool enabling different measurement geometries suited for transmission measurements, conventional XRF, ARXRF, etc. The chamber was specifically designed for attaching all kinds of laboratory X-ray sources for the soft and hard X-ray ranges as well as various detection systems. In detail, a setup for ARXRF using an X-ray tube with a polycapillary X-ray lens as source is presented. For such a type of setup, both the spectral and lateral characterizations of the radiation field are crucial for quantitative ARXRF measurements. The characterization is validated with the help of a stratified validation sample.

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

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vekemans, Bart [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Verhaeven, Eddy [Antwerp University, Faculty of Design Sciences, Mutsaardstraat 31, B-2000 Antwerpen (Belgium); Tack, Pieter; De Wolf, Robin; Garrevoet, Jan [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium)

    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. - Highlights: • New X-ray fluorescence and X-ray diffraction instrument for non-destructive analysis • Commercially available, mobile system • One of the lightest and most compact of its kind • Characterization, data acquisition and analysis are performed. • Results of measurements on pigment model samples and cultural heritage materials.

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

    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. - Highlights: • New X-ray fluorescence and X-ray diffraction instrument for non-destructive analysis • Commercially available, mobile system • One of the lightest and most compact of its kind • Characterization, data acquisition and analysis are performed. • Results of measurements on pigment model samples and cultural heritage materials

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

    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

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

    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.

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

    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

  4. Study of uranium contamination of ground water in Punjab using X-ray fluorescence technique

    A number of reports have appeared in public media about uranium ingestion being a possible cause for cancer and increased birth rate abnormalities among children in the Malwa region of Punjab state in India. These reports link problems like cancer and Autism, with the presence of uranium in the ground waters of Malwa region. The concentration of uranium in drinking water from sources as varied as ground water, canal water supply and reverse osmosis system have been investigated using X-ray fluorescence technique. Samples from the thermal power plants in the regions and nearby ground waters were also analyzed to identify the source of contamination. The samples were collected with assistance of the officials from the Government of Punjab. More than half a litre of each of the water samples was dried at 60 deg-80 deg in an oven. Residue was collected using larger quantities of water samples in case of RO water samples. The elemental analysis of the residue was carried out using the Energy-Dispersive X-Ray Fluorescence (EDXRF) spectrometer consisting of an 42Mo-anode X-ray tube (Panalytical, 2.5 kW) as an excitation source and a Si(Li) detector. A combination of selective absorbers of 30Zn, 38Sr, and 39Y was used in the incident beam for improving the detection limit for Uranium by reducing the background and removing the 42Mo K X-rays. The detection limit in ppb/litre depends upon the amount of residue

  5. Analyses of archaeological pottery samples using X-ray fluorescence technique for provenance study

    Archaeological artifacts reveal information on past human activities, artifact preparation technology, art and possible trade. Ceramics are the most stable and abundant material in archaeological context. Pottery is the most abundant tracers in all archaeological excavations. Compared to major elements, elements present at trace concentrations levels are source specific and they maintain same concentration levels in source clay as well as finished products e.g., fired clay potteries. As it is difficult to find out exact source or origin, provenance study is carried out first to establish whether objects under study are from the same or different sources/origin. Various analytical techniques like instrumental neutron activation analysis (INAA), Ion beam analysis (IBA) and X-ray fluorescence (XRF) have been used for obtaining elemental concentrations in archaeological potteries. Portable X-ray fluorescence (pXRF) spectrometry provides a non-destructive means for elemental characterization of a wide range of archaeological materials. Ten archaeological pottery samples were collected from Kottapuram, Kerala under the supervision of archaeological survey of India. Portable X-ray fluorescence (pXRF) spectrometry using a handheld Olympus Innov-X Delta XRF device, ACD BARC, has been used for chemical characterization of the pottery samples. The instrument is equipped with the Delta Rhodium (Rh) anode X-Ray tube and uses a Silicon Drift Detector (resolution <200 eV at 5.95 keV Mn Kα X-ray). NIST 2781 SRM was analyzed for quality control purpose. Ten elements namely Fe, Ti, Mn, Co, Cu, Zn, Pb, Zr, Mo and Se were chosen for cluster analysis and their concentration values were utilized for multivariate statistical analysis using WinSTAT 9.0

  6. Oscillating dipole model for the X-ray standing wave enhanced fluorescence in periodic multilayers

    André, Jean-Michel; Jonnard, Philippe

    2013-01-01

    Periodic multilayers give rise to enhanced X-ray fluorescence when a regime of standing waves occurs within the structure. This regime may concern the primary radiation used to induce the fluorescence, the secondary radiation of fluorescence or both of them. Until now, existing models only dealt with standing wave regime of primary radiation. We present a theoretical approach based on the oscillating dipole model and the coupled-wave theory that can treat efficiently any standing wave regime. We compare our simulations to experimental data available in the literature.

  7. Correction method for self-absorption effects of fluorescence x-ray absorption near-edge structure on multilayer samples

    It is well known that fluorescence x-ray absorption spectroscopy suffers from the self-absorption effects for thick and concentrated samples. In this study, a simple correction method is provided for correcting the self-absorption effects of fluorescence x-ray absorption near edge structure (XANES) spectrum for multilayer samples. This method is validated by application on fluorescence XANES spectra for a Cr/C multilayer measured at different incidence angles. The errors produced by the self-absorption effects for the measured fluorescence x-ray absorption spectra without corrections are also estimated and discussed. (paper)

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

    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.

  9. 3D Micro-PIXE at atmospheric pressure: A new tool for the investigation of art and archaeological objects

    The paper describes a novel experiment characterized by the development of a confocal geometry in an external Micro-PIXE set-up. The position of X-ray optics in front of the X-ray detector and its proper alignment with respect to the proton micro-beam focus provided the possibility of carrying out 3D Micro-PIXE analysis. As a first application, depth intensity profiles of the major elements that compose the patina layer of a quaternary bronze alloy were measured. A simulation approach of the 3D Micro-PIXE data deduced elemental concentration profiles in rather good agreement with corresponding results obtained by electron probe micro-analysis from a cross-sectioned patina sample. With its non-destructive and depth-resolving properties, as well as its feasibility in atmospheric pressure, 3D Micro-PIXE seems especially suited for investigations in the field of cultural heritage

  10. Laser 3D micro-manufacturing

    Piqué, Alberto; Auyeung, Raymond C. Y.; Kim, Heungsoo; Charipar, Nicholas A.; Mathews, Scott A.

    2016-06-01

    Laser-based materials processing techniques are gaining widespread use in micro-manufacturing applications. The use of laser microfabrication techniques enables the processing of micro- and nanostructures from a wide range of materials and geometries without the need for masking and etching steps commonly associated with photolithography. This review aims to describe the broad applications space covered by laser-based micro- and nanoprocessing techniques and the benefits offered by the use of lasers in micro-manufacturing processes. Given their non-lithographic nature, these processes are also referred to as laser direct-write and constitute some of the earliest demonstrations of 3D printing or additive manufacturing at the microscale. As this review will show, the use of lasers enables precise control of the various types of processing steps—from subtractive to additive—over a wide range of scales with an extensive materials palette. Overall, laser-based direct-write techniques offer multiple modes of operation including the removal (via ablative processes) and addition (via photopolymerization or printing) of most classes of materials using the same equipment in many cases. The versatility provided by these multi-function, multi-material and multi-scale laser micro-manufacturing processes cannot be matched by photolithography nor with other direct-write microfabrication techniques and offer unique opportunities for current and future 3D micro-manufacturing applications.

  11. Monitoring the mass of UF6 gas and uranium deposits in aluminium pipes using X-ray fluorescence and X-ray transmission gauges

    In order to determine the enrichment of UF6 gas in centrifuge plant pipework it is necessary to measure the mass of the gas (pressure) and the mass per unit area of any uranium deposited on the pipe. This paper shows that it is possible to determine the pressure of the UF6 gas in pipes 120 mm in diameter using an energy-dispersive X-ray fluorescence spectrometer. Results are also given of transmission measurements made using a low power X-ray generator operated at two different applied voltages. A method of using the two measurements to determine the mass per unit area of deposited uranium is described. (author)

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

    Glans, P.; Gunnelin, K.; Guo, J. [Uppsala Univ. (Sweden)] [and others

    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.

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

    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.

  14. Application of the X-ray fluorescence analysis and X-ray diffraction in geochemical studies of the Pleistocene tills from Holy Cross Mountains

    Kubala-Kukuś, A.; Ludwikowska-Kȩdzia, M.; Banaś, D.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.

    2013-12-01

    X-ray fluorescence analysis methods (wavelength dispersive X-ray fluorescence analysis (WDXRF) and total reflection X-ray fluorescence (TXRF)) and X-ray powder diffraction (XRPD) have been applied in complementary geochemical studies of the Pleistocene till samples. The XRPD technique gave information about the mineral composition of the analyzed samples while the WDXRF and TXRF studies allowed the fast elemental analysis. The till samples were collected from different regions of Holy Cross Mountains (located in central Poland) which are still not unambiguously described in the context of the geochemical studies of the Quaternary sediments. The analysis was concentrated on the geochemical composition of the till samples both for materials occurring on the surface (characterized by continuous weathering processes) and for samples taken from core borehole. The overriding purpose of these studies is determination of the local lithotype of the tills and its lithologic and petrographic diagnostic properties, including the chemical composition of clay and minerals found in the clay. In the presented work the experimental sets up, sample preparation procedure and measurements programme will be discussed in details. Finally, the elemental and mineral compositions will be presented for studied different groups of the samples.

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

    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.

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

    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 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. (author)

  17. Total reflection X-Ray Fluorescence in medicine. Technique and applications

    The developments Total reflection X-Ray Fluorescence techniques is make the method appropriate for sample, accurate and precise analysis of heavy element in organic fluid and tissue in health related and pollutions problems, Application include analysis as an advantageous aid in drug synthesis and characterization, trace elements determination in amniotic fluid in fetus malformation studies, analysis of brain specimens and cerebrospinal fluid in central nervous system disorders, the influence of trace elements in cataract genesis and blood, body fluids and tissue drug level- monitoring. Accuracy, precision and detection limits attained in the analysis of platinum in minute amounts of serum from oncological pediatric patients undergoing chemotherapy which Pt-containing drugs shows Total reflection X-Ray Fluorescence could be used for routine analysis as an aid in clinical practice

  18. Determination of copper in geological materials by X-ray fluorescence

    X-ray fluorescence has been applied to the determination of copper content of geological materials in the concentration range of 0.01 to % CuO. A molybdenum target tube Is used, samples being presented in finely-ground powder form. Various methods for the correction for background and Instrumental copper interferences have been considered. To correct for matrix effects different tube scattered primary radiations have been tested as references or internal standards. MoK(41 - (C) provides the most suitable results. The use of influence empirical coefficients for the effect of iron on copper and of mass absorption coefficients has also been considered. For samples with a high content of lead, several procedures to correct for I t s influence have been investigated. Comparison between data obtained by X-ray fluorescence and wet-chemical techniques indicated good agreement. (Author) 6 refs

  19. Role of importance of X-ray fluorescence analysis of forensic samples

    Full text: In the field of forensic science, it is very important to investigate the evidential samples obtained at various crime scenes. X-ray fluorescence (XRF) is used widely in forensic science [1]. Its main strength is its non-destructive nature, thus preserving evidence [2, 3]. In this paper, we report the application of XRF to examine the evidences like purity gold and silver jewelry (Indian Ornaments), remnants of glass pieces and paint chips recovered from crime scenes. The experimental measurements on these samples have been made using X-ray fluorescence spectrometer (LAB Center XRF-1800) procured from Shimazdu Scientific Inst., USA. The results are explained in terms of quantitative/ qualitative analysis of trace elements. (author)

  20. X-ray fluorescence/Auger-electron coincidence spectroscopy of vacancy cascades in atomic argon

    Arp, U. [National Inst. of Standards and Technology, Gaithersburg, MD (United States). Electron and Optical Physics Div.; LeBrun, T.; Southworth, S.H.; Jung, M. [Argonne National Lab., IL (United States). Physics Div.; MacDonald, M.A. [E.P.S.R.C. Daresbury Lab., Warrington (United Kingdom)

    1996-12-01

    Argon L{sub 2.3}-M{sub 2.3}M{sub 2.3} Auger-electron spectra were measured in coincidence with K{alpha} fluorescent x-rays in studies of Ar K-shell vacancy decays at several photon energies above the K-threshold and on the 1s-4p resonance in atomic argon. The complex spectra recorded by conventional electron spectroscopy are greatly simplified when recorded in coincidence with fluorescent x-rays, allowing a more detailed analysis of the vacancy cascade process. The resulting coincidence spectra are compared with Hartree-Fock calculations which include shake-up transitions in the resonant case. Small energy shifts of the coincidence electron spectra are attributed to post-collision interaction with 1s photoelectrons.

  1. An evaluation of the x-ray-fluorescence analysis of rocks and silicates under routine conditions

    This report correlates the analytical results obtained by four laboratories using X-ray-fluorescence analysis on ten reference silicate samples that were incorporated in the analytical programmes required by the Geological Survey of the Republic of South Africa over a five-year period. The results and their statistical treatment are given, together with a comparison of the results for similar material issued by the Centre de Recherches Petrographiques et Geochimiques and the British Ceramic Research Association using wet-chemical methods. This study shows that the analysis, by X-ray-fluorescence measurement, of rocks and silicate samples for the commonly determined constituents is more precise than analysis by classical wet-chemical procedures

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

    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. Correlated imaging of living biological cells with a soft X-ray microscope and a fluorescence microscope

    Soft X-ray microscope is a very powerful tool to observe cellular organelles of living biological. However the inner structures are very complicated and it is difficult to identify the organelles obtained with the soft X-ray microscopes. We have proposed a correlated imaging with a soft X-ray microscope and a fluorescence microscope that is to observe the same biological cells with the both microscopes at the same time. (author)

  4. Zinc content determination in rice and other agricultural products by X-ray fluorescence

    The Zn content in regular consumption foodstuff (rice, some vegetables and roots) in Cuba is reported. Concentrations are determined by X-Ray Fluorescence analysis using a set of organic standards doped with Zn. The accuracy of the analytical procedure was validated using the Certified Reference Materials IAEA 393 and y MA-B-3/TM. The obtained results show rice as the major Zn bioaccumulator of the studied agricultural products and the main Zn source in Cuban human diet. (author)

  5. Development and state of total reflection X-ray fluorescence analysis

    Since the first application of total reflection in X-ray fluorescence analysis at the beginning of the 1970's this method has been subject to continual modifications and improvements and has frequently competed with NAA, ICP and AAS as a micro-analysis process for traces in the nanogram and picogram range. A survey is given of the many applications published in the literature, particularly of applications in environmental research practised at the GKSS Research Centre. (RB)

  6. Multielemental analysis of surface sediments in Havana bay (Cuba) using X-ray fluorescence

    Multielemental Analysis was performed in Superficial Sediments in Havana Bay. Twenty one samples were analysed by Dispersive Energy X- Ray Fluorescence using an spectrometer based on Si (Li) semiconductor detector an a 109 Cd source. The results showed a similar behaviour in the levels of contamination related with neutron activation analysis. The data suggest that an anthropogenic input into the bay from domestic sewage and industries occurred. (Full text)

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

    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 microg of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. PMID:18960464

  8. Examination of the trace element content of beetroot by X-ray fluorescence analysis

    The paper deals with the determination of Mn, Fe, Cu, Zn, Br, Rb, Sr, Mo concentration in beetroot by energy dispersive X-ray fluorescence method. The exciting source was 125I with 555 MBq activity. For the analysis Si(Li) semiconductor detectors were applied and for the data processing a minicomputer (type HP 9825 A) was used. Results are given in tabulated form. (Sz.J.)

  9. Precision measurement of Fe concentration in dolomites using radioisotope x-ray fluorescence

    A series of dolomite bore hole samples were analyzed for their iron content using radioisotope x-ray fluorescence. A precision of +-0.1%, as specified for oil and gas exploration was met using a nondestructive sample preparation technique, energy dispersive detector, sup(109)Cd source and a micro-computer based data acquisition and reduction system. Sample and standard preparation procedures are discussed. (author)

  10. Quantitatively Imaging Chromosomes by Correlated Cryo-Fluorescence and Soft X-Ray Tomographies

    Smith, Elizabeth A.; McDermott, Gerry; Do, Myan; Leung, Karen; Panning, Barbara; Le Gros, Mark A.; Larabell, Carolyn A.

    2014-01-01

    Soft x-ray tomography (SXT) is increasingly being recognized as a valuable method for visualizing and quantifying the ultrastructure of cryopreserved cells. Here, we describe the combination of SXT with cryogenic confocal fluorescence tomography (CFT). This correlative approach allows the incorporation of molecular localization data, with isotropic precision, into high-resolution three-dimensional (3-D) SXT reconstructions of the cell. CFT data are acquired first using a cryogenically adapted...

  11. Modelling of Grazing Incidence X-Ray Fluorescence (GIXRF) for surface layer characterisation.

    Brigidi, Fabio

    2015-01-01

    GIXRF (Grazing incidence X-Ray Fluorescence) is an analytical technique with high potential in the study of depth profiles and in the characterization of thin layered structures. To extract information from a GIXRF measurement and determine the layer composition it is necessary to compare the experimental data with simulation. However at the moment this thesis has been written, there is no software widely recognized from the scientific community as the reference software for the analysis. ...

  12. Determination of potassium concentration in organic samples by means of x-ray fluorescence analysis

    By means of x-ray fluorescence analysis and the inner standard method using KH2PO4 as the added chemical compound, potassium concentration of roots, stems , leaf, flowers and grains from Quinua (Chenopodium Quinoa Willd). which was previously treated with a nitrogen ed fertilizers has been determined taking into account the increasing effect the average atomic number due to used standard. Experimental errors are lower than 10 %

  13. Energy-dispersive X-ray fluorescence analysis of cerium in ferrosilicon

    The cerium was determined in ferrosilicon samples by energy-dispersive X-ray fluorescence techniques (XRF) techniques, with a secondary target of gadolinium. The methods employed were: comparison and linear regression with reference materials with cerium concentration between 0.4 and 1.0%. The samples were prepared in the form of pellets and the analytical results are reported as an average of five determinations with a confidence limits at 95% probability. (Author)

  14. Chemical composition of soils and biosolid by X-ray fluorescence technique

    The objective of the present work was to investigate the chemical composition of biosolid and soil treated with biosolid using the energy dispersive X-ray fluorescence. The elements Br, Co, Cr, Cu, Fe, Ga, Mn, Ni, Pb, Se, Sr, Ti and Zn were quantified and the results had been compared with Brazilian legislation. The Ni, Cu, Cr and Zn amounts were below the maximum values allowed. (author)

  15. Criteria to stablish an absolute semiquantitative analytic method by x-ray fluorescence

    This work had been developed by fluorescence x-ray laboratory of Nuclear Studies Centre form Ecuador, it pretent to stablish an appropiate discernement of a FRX spectrum to know the concentration range form sample elements, minerals principaly, submit to a FRX. The study tries to stablish the best way to calibration the instruments like the adecuate samples preparation to do the analysis by FRX

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

    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.

  17. Elemental analysis of hair samples using energy dispersive X-ray fluorescence and atomic absorption spectroscopy

    Elemental analysis of hair samples was performed using energy dispersive X-ray fluorescence. The ion exchange preconcentration technique was employed. The capacity of the exchanger used-cellulose hyphan at different pH was investigated to determine the optimum pH for the resin. The capacity of the resin to take up elements of interest from mixed solutions was also analysed using atomic absorption spectroscopy. (author)

  18. Determination of low concentrations of thorium in geological materials by X-ray fluorescence

    An X-ray fluorescence method for the determination of thorium in geological samples down to 2 ppm ThO2 has been developed. To achieve this determination limit an exposed area of the sample 42.5 mm in diameter is used, working with a molybdenum target tube operated at 90 kV and 30 m A. Corrections for background and line interference of the Rb Kα radiation have been carefully considered and empirical correction coefficients calculated. (Author) 3 refs

  19. Radioisotope induced X-ray fluorescence analysis of cereal grains and flour

    Radioisotope-induced X-ray fluorescence analysis is a rather simple and easy method for investigating ashed plant material. In order to reduce matrix effects thin samples of 2 mg/cm2 are analysed to obtain a reasonable compromise between maximum sensitivity and the lowest possible absorption effects. Concentrations are determined by standard addition method. An accuracy of 6-8% can be achieved. As an application analytical results are given for whole grains of several sorts of wheat. (author)

  20. Radioisotope induced X-ray fluorescence analysis of cereal grains and flour

    Radioisotope induced X-ray fluorescence analysis is a rather simple and convenient method for investigating ashed plant materials. In other to reduce matrix effects, thin samples (2 mg/cm2) are analyzed to obtain a reasonable compromise between maximum sensitivity and the lowest possible absorption effects. Concentrations are determined by standard addition method. A precision of 6-8% can be achieved. As an application, analytical results are given for whole grains of several sorts of wheat. (author)

  1. Determination of pollutants in dwellings by neutron activation analysis and x-ray fluorescence

    Metallic pollutants were measured in dwellings in Mexico city by instrumental neutron activation analysis (INAA) and x-ray fluorescence techniques. Monitoring was performed in the west side of the city and in the winter season. In general the average concentration of contaminants collected, when compared with average concentrations reported in a previous paper, have increased with time and in the particular case of lead and mercury some samples are above the indicative WHO maximum levels. (author)

  2. Quantitative determination of uranium in organic solution by X-ray fluorescence

    An X-ray fluorescent method for the determination of uranium in tributilphosphate-kerosene-nitriacid solution has been developed. Chemical properties of the matrix elements were studied in order to select a convenient procedure to determine samples and standards on the same way. The method avoids the destruction of the organic material and has proved to be very useful for the fast control of uranium concentration. (Author)

  3. X-ray fluorescence analysis of ancient and medieval brass artifacts from south Moravia

    This paper deals with an investigation of archeological finds using X-ray fluorescence analysis and microanalysis. The main aim of the investigation was to prove the production of brass in the South Moravian Region (part of the Czech Republic) in former times. The probable brass production technology is described. Various objects dating back to Antiquity and to the Middle Ages were investigated using two X-ray fluorescence systems, and the results of the analyses are discussed. The measurements showed, e.g., that fragments of Roman scale armor and a belt fitting dating back to Antiquity were made of brass. Brass was also identified on the surfaces of various ancient and medieval molds and melting pots. - Highlights: ► Semiquantitative X-ray fluorescence analysis of archeological finds. ► Two different gilding techniques of a brass belt terminal found in Brno. ► Use of brass before the Great Moravian period. ► Evidence of brass casting in the 12th century in Brno.

  4. X-ray fluorescence analysis of ancient and medieval brass artifacts from south Moravia

    Hlozek, M. [Methodical Centre of Conservation-Technical Museum in Brno, Purkynova 105, 612 00 Brno (Czech Republic); Komoroczy, B. [Institute of Archeology of the Academy of Science of the Czech Republic, Kralovopolska 147, 612 00 Brno (Czech Republic); Trojek, T., E-mail: tomas.trojek@fjfi.cvut.cz [Department of Dosimetry and Application of Ionizing Radiation, Czech Technical University in Prague, Brehova 7, 115 19 Praha 1 (Czech Republic)

    2012-07-15

    This paper deals with an investigation of archeological finds using X-ray fluorescence analysis and microanalysis. The main aim of the investigation was to prove the production of brass in the South Moravian Region (part of the Czech Republic) in former times. The probable brass production technology is described. Various objects dating back to Antiquity and to the Middle Ages were investigated using two X-ray fluorescence systems, and the results of the analyses are discussed. The measurements showed, e.g., that fragments of Roman scale armor and a belt fitting dating back to Antiquity were made of brass. Brass was also identified on the surfaces of various ancient and medieval molds and melting pots. - Highlights: Black-Right-Pointing-Pointer Semiquantitative X-ray fluorescence analysis of archeological finds. Black-Right-Pointing-Pointer Two different gilding techniques of a brass belt terminal found in Brno. Black-Right-Pointing-Pointer Use of brass before the Great Moravian period. Black-Right-Pointing-Pointer Evidence of brass casting in the 12th century in Brno.

  5. X-ray fluorescence analysis in application for study of human brain tissue and body fluids

    Thin slices of human brain tissue and body fluids were investigated using Energy Dispersive X-Ray Fluorescence (EDXRF) spectrometry. Distribution of elements in brain tissue samples was studied using Microbeam X-Ray Fluorescence (MXRF) method. Total Reflection X-Ray fluorescence (TXRF) analysis was applied for determination of elemental contens in cerebrospinal fluid, serum and whole blood. The main goal of the study was to optimize analytical procedures for investigation of biomedical specimens using EDXRF method. MXRF method is useful for investigation of P, S, Cl, K, Ca and Fe. Moreover, it can be also applied for distinguishing between white and gray matter of the human brain. Two sample preparation methods were applied in TXRF spectrometry with respect to detection limit. In the first method the body fluids were analysed without any sample preparation. The other measurements were performed for the body fluids digested with nitric acid. For both methods gallium was used as an internal standard. Accuracy of the TXRF method was assessed using Certified Reference Material, A-13 (freeze-dried animal blood). High sensitivity of TXRF and proper sample preparation allowed to detect wide spectrum of elements between Cl and Sr. Faster and easier first sample preparation method allowed to detect elements including volatile ones like Cl or Br whereas digestion of fluids with nitric acid improved the detection limits significantly. Elemental analysis of thin brain tissue samples and body fluids will be applied for study of role of trace elements in selected neurological diseases. (author)

  6. Clumpy tori around type II active galactic nuclei as revealed by X-ray fluorescent lines

    Liu, Jiren; Liu, Yuan; Li, Xiaobo; Xu, Weiwei; Gou, Lijun; Cheng, Cheng

    2016-06-01

    The reflection spectrum of a torus around an active galactic nucleus (AGN) is characterized by X-ray fluorescent lines, which are most prominent for type II AGNs. A clumpy torus allows photons reflected from the back-side of the torus to leak through the front regions that are free of obscuration. The observed X-ray fluorescent lines are therefore sensitive to the clumpiness of the torus. We analysed a sample of type II AGNs observed with the Chandra High Energy Transmission Grating Spectrometer (HETGS), and measured the fluxes for the Si Kα and Fe Kα lines. The measured Fe Kα/Si Kα ratios, spanning a range between 5 and 60, are far smaller than the ratios predicted from simulations of smooth tori, indicating that the tori of the studied sources have clumpy distributions rather than smooth ones. We compared the measured Fe Kα/Si Kα ratios with simulation results of clumpy tori. The Circinus galaxy has a Fe Kα/Si Kα ratio of ˜60, which is close to the simulation results for N = 5, where N is the average number of clumps along the line of sight. The Fe Kα/Si Kα ratios of the other sources are all below the simulation results for N = 2. Overall, this shows that the non-Fe fluorescent lines in the soft X-ray band are a potentially powerful probe of the clumpiness of tori around AGNs.

  7. Fluorescence x-ray standing wave study on (AlAs)(GaAs) superlattices

    Lessmann, A; Munkholm, A; Schuster, M; Riechert, H; Materlik, G

    1999-01-01

    X-ray standing waves (XSW) were used to investigate the structure of molecular beam epitaxy (MBE) grown (AlAs) sub 3 (GaAs) sub 7 short-period superlattices (SPSL). The modulation of the Al K, As L, and Ga L x-ray fluorescence induced by XSW was measured at the zero-order superlattice (SL) satellite (AlAs)(GaAs)(004,0) and the GaAs(004) substrate Bragg reflection. From the shape of the fluorescence yield modulations and the diffraction pattern, a model of the interfaces is derived by comparing the experimental data with dynamical calculations of the x-ray wave field distribution and reflectivity. A straightforward analysis of the fluorescence measurements at the SL satellite shows that in AlAs layers a high crystalline order is established, whereas in GaAs layers a fraction of the Ga and As atoms is not on ideal lattice sites, but is displaced towards the substrate. The data can be explained by a model in which, at each AlAs/GaAs interface of the GaAs layers, two Ga atom planes are displaced by 0.035 nm and 0...

  8. A set-up of micro-X-ray fluorescence system based on polycapillary X-ray optics and applications for archaeology

    The paper concerns in the structures, performances and characteristics and applications for archaeology of a new micro-X-ray fluorescence system based on rotating anode X-ray generator and polycapillary X-ray optics. The polycapillary X-ray optics used here can focus the primary X-ray beam down to some tens of micrometers in diameters that allows for non-destructive and local analysis of sub-mm samples with minor/ trace level sensitivity. In order to prove the potentials of this instrument used in archaeology, a piece of Chinese ancient blue and white porcelain produced in Ming Dynasty was analyzed. The results show that intensities of Mn-Kα, Co-Kα are variable in agree with the thick of blue glaze. The correlation analysis indicates the Mn and Co have the best correlations. So, the concentrations or ratios of Mn and Co are crucial to determine the provenance and identify from a fake one of Chinese ancient blue and white porcelain. (authors)

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

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

    2014-09-01

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

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

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

  11. Analysis of metal in organic compound used in the agriculture by x-ray fluorescence

    Using energy dispersive X-ray fluorescence analysis with an X-ray tube filtered with Ti. It was possible to determine the concentration of the elements at ppm level of several elements: K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn As, Rb, Sr, Y, Zr, and Pb in two types of organic compound enough used in the agriculture: organic compound of urban garbage (Fertilurb) and birds manure. The experimental setup is composed of: X-ray tube (Oxford, 30 kV, 50 mA and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray beam is quasi-monochromatic by using Ti filter. The samples were prepared in pellet form with superficial density in the range of 100 mg/cm2. The fundamental parameter method was used in order to verify the elemental concentration. The radiation transmission method was going used to the radiation absorption effects correction in the samples

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

    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. PMID:22483897

  13. Investigation of drug loading behavior of dendrimers nano-vectors with synchrotron radiation hard X-ray fluorescence analysis

    Background: Synchrotron Radiation X-ray fluorescence analysis is an advanced method of quantitative elemental analysis. It is a scientific platform for life science, material science, and environmental science. Purpose: In this present study, the drug loading behavior of dendrimers nano-vectors was investigated by using the method of Synchrotron Radiation X-ray fluorescence analysis. Methods: The copper (Ⅱ) ions were loaded into acetyl-modified generation 5(G5) PAMAM dendrimers. We monitored and imaged the distribution of copper in A549 cell by Shanghai Synchrotron Radiation Facility (SSRF) to observe the cellular uptake of copper-dendrimers conjugates. Results: The results of hard X-ray fluorescence mapping showed a stronger fluorescence of Cu in the cells treated with G5-Ac-Cu than that of control. Conclusions: This investigation provided a method of using synchrotron radiation X-ray fluorescence analysis to study the drug loading behavior of dendrimers. (authors)

  14. Development of confocal 3D micro-XRF spectrometer with dual Cr-Mo excitation

    A new 3D micro-XRF instrument based on a confocal setup using two independent poly-capillary x-ray lenses and two x-ray sources (Cr and Mo targets) was developed. A full poly-capillary x-ray lens was attached to each x-ray tube. Another half poly-capillary lens was attached to a silicon drift x-ray detector (SDD). The focal spots of the three lenses were adjusted to a common position. The depth resolutions that were evaluated by use of a 10-μm thick Au foil were approximately 90 μm for the x-ray energy of Au Lα. The effects of the dual Cr-Mo x-ray beam excitation were investigated. It was confirmed that the XRF intensity of light elements was increased by applying the Cr-target x-ray tube in a confocal configuration. In the proposed confocal configuration, 3D elemental mapping of the major elements of an amaranth seed was performed nondestructively at ambient air pressure. Each element of the seed showed different mapping images in the different depth layers. (authors)

  15. Application of energy dispersive X-ray fluorescence for the determination of selenium in blood and tissue

    The application of low-power transmission X-ray tubes with Mo and Ag targets for the determination of trace concentration of selenium in blood and tissue has been described. The energy dispersive X-ray fluorescence method with the use of Si(Li) detector gives the possibility of selenium determination in ppb level. (author)

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

    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.

  17. FLUORESCENT X-RAY-ANALYSIS OF URANIUM USING INTERNAL STANDARD AND FILTER METHODS

    Arikan, P.; Özmen, A.

    1987-01-01

    Interna1 standard and filter methods for fluorescent X-ray analysis of uranium in ores are investigated. In the first method, successful application of strontium K-X internal standard line for uranium L-X analyte line is carried out. Standardization with strontium eliminated the absorption-enhancement effect in analysis. In the second method, strontium and thorium are chosen as filters for uranium L-X and K-X fluorescent rays respectively. Attenuation (Hull) filters are used to remove ULβ, UK...

  18. An X-ray fluorescence system for measuring trace element concentrations in breast tissue

    X-ray fluorescence is being used as a technique for measuring concentrations of trace elements in breast tissue samples, both healthy and pathological. The aim is to establish the levels of some trace elements in normal tissue and subsequently compare with those in cancerous, as there are indications that there is a correlation between elevated concentrations of some elements in breast tissue and development of cancer. As a first step of these pilot studies we are investigating four such elements, Fe, Ca, Zn and Cu, but we plan to expand the study to include Se and Rb. The tissue samples are kept at -85 deg C and are stored in thin walled polypropylene tubes of 8 mm diameter, which can be unsealed from one end so that the samples can be exposed to the beam. The experimental set-up consists of a high output tungsten target X-ray source, a secondary target from which characteristic X-rays of an appropriate energy are produced, a sample holder and a Si detector. The geometry is highly collimated in order to promote a high signal to noise ratio for the fluorescence X-rays from the sample. The measurements will be compared to reference solutions of various concentrations of the elements of interest. The aim is to establish a calibration curve for each element, from which the correlation between fluorescence yield and element concentration can be extracted, leading to actual trace element levels in tissue. We hope to prove the feasibility of monitoring elements in levels normally found in breast tissue, using this XRF technique. We plan to show results referring both to normal and neoplastic tissue, stating levels of as many trace elements as possible. We should also be able to present minimum detectable levels regarding every element investigated with this system, as well as have propositions for further optimising the performance of the technique. (author)

  19. The use of portable X-ray Fluorescence Spectrometry (PXRFS) for clinical practices

    In the last years X-Ray Fluorescence (X RF) technique has been applied to clinical finality at IPEN/CNEN-S P, in collaboration with blood banks and research centers from Brazil. The major advantage for using this analytic technique for chemistry clinical is the viability to use small quantities of blood (25 to 100μL) comparatively to conventional analyses preformed using serum (at least 500 μL to 10 m L). Besides, the execution is faster and the procedure is not destructive. Now, we intend to check the viability of using a portable X- Ray Fluorescence Spectrometry (PXRFS) for clinical blood examination. In this study the biological samples came from Blood Banks of Sao Paulo city (Brazil). Each sample was collected in a vacuum plastic tube (without anticoagulants) attached to the donors arm and, immediately after the collection exactly, 100 μ L of whole blood was transferred to the filter paper (Whatman, n 41) using a calibrated micropipette and it was dried for few minutes using an infrared lamp. Samples were prepared in duplicate. The X RF analysis was performed using Mini X spectrometer from Amptek, model X-123 Sdd with Ag X-ray tube. The characteristics X-ray fluorescent intensities (Kα lines) were measured with a Si detector (Si Drift 25 m m2 x 500 μm / 0.5 mil) Be (window / 1.5) and biological samples were irradiated for 300s using 30 kV and 5 μA excitation. The quantitative analysis was performed using WINAXIL software program. We intend to stimulate the use of this small spectrometry as an alternative for diagnostic of the clinical diseases that have high prevalence in Brazilian population

  20. Development of soil reference materials containing hazardous metals for X-ray fluorescence analysis

    Soil standards containing hazardous metals (Cr, As, Se, Cd, Hg, and Pb) were developed for X-ray fluorescence analysis (XRF). Standard soil was prepared by adding appropriate amount of aqueous standard solutions to the base soil (brown forest soil; Fukuoka, Japan) and then drying and homogenizing. The analytical lines were CrKα, AsKα, SeKα, CdKα, HgLα and PbLβ accompanied by the corrections for the overlapping of SeKβ to PbLβ and PbLα to AsKα. Specimens for XRF analysis were prepared by a powder briquette molded in the 23 mmφ of an Al ring with 300 kgf cm-2. The homogeneity and durability of the standards were checked by the fluorescent X-ray intensities and the statistical errors for briquette samples. Each of the intensities varied slightly, and the relative standard deviations of the XRF intensities of Cr, As, Se, Cd, and Pb in 10 briquettes were less than 0.3%. The X-ray resistant performance of the soil standards was checked by the repetitive irradiation of 4 kW X-ray. The fluorescence intensities of Cr, As, Se, Cd, and Pb showed constant values for 240 min of irradiation. The HgLα intensity was almost constant for 60 min of irradiation in air. The calibration curves constructed proposed standards showing good linearity under 3000 mg kg-1 for Cr, As, Se, Cd, Pb, and 300 mg kg-1 for Hg. The lower limits of detection were 0.84 - 2.7 mg kg-1 (author)

  1. Application of the X-ray fluorescence analysis and X-ray diffraction in geochemical studies of the Pleistocene tills from Holy Cross Mountains

    X-ray fluorescence analysis methods (wavelength dispersive X-ray fluorescence analysis (WDXRF) and total reflection X-ray fluorescence (TXRF)) and X-ray powder diffraction (XRPD) have been applied in complementary geochemical studies of the Pleistocene till samples. The XRPD technique gave information about the mineral composition of the analyzed samples while the WDXRF and TXRF studies allowed the fast elemental analysis. The till samples were collected from different regions of Holy Cross Mountains (located in central Poland) which are still not unambiguously described in the context of the geochemical studies of the Quaternary sediments. The analysis was concentrated on the geochemical composition of the till samples both for materials occurring on the surface (characterized by continuous weathering processes) and for samples taken from core borehole. The overriding purpose of these studies is determination of the local lithotype of the tills and its lithologic and petrographic diagnostic properties, including the chemical composition of clay and minerals found in the clay. In the presented work the experimental sets up, sample preparation procedure and measurements programme will be discussed in details. Finally, the elemental and mineral compositions will be presented for studied different groups of the samples. - Highlights: • XRF analysis and X-ray diffraction used in studies of the till samples. • The till samples were collected from different regions of Holy Cross Mountains. • The analysis concentrates both on the samples from surface and from core borehole. • The purpose is determination of the local lithotype of the tills. • The experimental setup, sample preparation, measurements and results are discussed

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

    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 μm 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 107atoms/cm2 level in the next few years. Current commercial systems using rotating anode x-ray sources presently routinely operate with a sensitivity level of around 1010 atoms/cm2 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

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

    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

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

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

    2016-07-01

    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. Details of the device design, data analysis and opportunities for further sensitivity improvement are described. PMID:27359138

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

    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.

  6. Dose distribution calculation for in-vivo X-ray fluorescence scanning

    In-vivo X-ray fluorescence constitutes a useful and accurate technique, worldwide established for constituent elementary distribution assessment. Actually, concentration distributions of arbitrary user-selected elements can be achieved along sample surface with the aim of identifying and simultaneously quantifying every constituent element. The method is based on the use of a collimated X-ray beam reaching the sample. However, one common drawback for considering the application of this technique for routine clinical examinations was the lack of information about associated dose delivery. This work presents a complete study of the dose distribution resulting from an in-vivo X-ray fluorescence scanning for quantifying biohazard materials on human hands. Absorbed dose has been estimated by means of dosimetric models specifically developed to this aim. In addition, complete dose distributions have been obtained by means of full radiation transport calculations in based on stochastic Monte Carlo techniques. A dedicated subroutine has been developed using the Penelope 2008 main code also integrated with dedicated programs -Mat Lab supported- for 3 dimensional dose distribution visualization. The obtained results show very good agreement between approximate analytical models and full descriptions by means of Monte Carlo simulations. (Author)

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

    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

  8. Resonance fluorescence in ultrafast and intense x-ray free-electron-laser pulses

    Cavaletto, S M; Harman, Z; Kanter, E P; Southworth, S H; Young, L; Keitel, C H

    2012-01-01

    The spectrum of resonance fluorescence is calculated for a two-level system excited by an intense, ultrashort x-ray pulse made available for instance by free-electron lasers such as the Linac Coherent Light Source (LCLS). We allow for inner-shell hole decay widths and destruction of the system by further photoionization. This two-level description is employed to model neon cations strongly driven by x rays tuned to the $1s 2p^{-1}\\rightarrow 1s^{-1} 2p$ transition at 848 eV; the x rays induce Rabi oscillations which are so fast that they compete with Ne $1s$-hole decay. We predict resonance fluorescence spectra for two different scenarios: first, chaotic pulses based on the Self Amplified Spontaneous Emission principle, like those presently generated at XFEL facilities and, second, Gaussian pulses which will become available in the foreseeable future with self-seeding techniques. As an example of the exciting opportunities deriving from the use of seeding methods, we predict, in spite of above obstacles, the ...

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

    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.

  10. X-ray fluorescence microtomography on a SiC nuclear fuel shell

    TRISO fuel particles contain a small kernel of nuclear fuel encapsulated by alternating layers of C and a barrier layer of SiC. The TRISO fuel particle is used in an advanced nuclear fuel where the SiC shell provides the primary barrier for radioactive elements in the kernel. The performance of this barrier is key to containment. The authors have used x-ray fluorescence microtomography to measure the trace element distribution in a SiC shell. Prior to the measurements the nuclear fuel and C layers were leached from the particle. The shell was then encapsulated by kapton tape to simplify handling. The shell was mounted on a glass fiber and measurements were made with an ∼ 1 x 3 microm2 x-ray probe on beamline 2-ID at the APS. The distribution of trace elements in the SiC shell was reconstructed after correcting the data for artifacts arising from absorption and scattering off the kapton tape. The observed trace elements are distributed in small < 1 microm regions through the SiC shell. The trace elements can be attributed to radiation enhanced diffusion of elements in the kernel or to trace elements introduced during fabrication. X-ray fluorescence microtomography is an ideal tool for this work because it is a penetrating nondestructive probe sensitive to trace elements in a low Z matrix and because it provides a picture of the elemental distribution in the shell

  11. Dose distribution calculation for in-vivo X-ray fluorescence scanning

    Figueroa, R. G. [Universidad de la Frontera, Departamento de Ciencias Fisicas, Av. Francisco Salazar 1145, Temuco 4811230, Araucania (Chile); Lozano, E. [Instituto Nacional del Cancer, Unidad de Fisica Medica, Av. Profesor Zanartu 1010, Santiago (Chile); Valente, M., E-mail: figueror@ufro.cl [Consejo Nacional de Investigaciones Cientificas y Tecnicas, Av. Ravadavia 1917, C1033AAJ, Buenos Aires (Argentina)

    2013-08-01

    In-vivo X-ray fluorescence constitutes a useful and accurate technique, worldwide established for constituent elementary distribution assessment. Actually, concentration distributions of arbitrary user-selected elements can be achieved along sample surface with the aim of identifying and simultaneously quantifying every constituent element. The method is based on the use of a collimated X-ray beam reaching the sample. However, one common drawback for considering the application of this technique for routine clinical examinations was the lack of information about associated dose delivery. This work presents a complete study of the dose distribution resulting from an in-vivo X-ray fluorescence scanning for quantifying biohazard materials on human hands. Absorbed dose has been estimated by means of dosimetric models specifically developed to this aim. In addition, complete dose distributions have been obtained by means of full radiation transport calculations in based on stochastic Monte Carlo techniques. A dedicated subroutine has been developed using the Penelope 2008 main code also integrated with dedicated programs -Mat Lab supported- for 3 dimensional dose distribution visualization. The obtained results show very good agreement between approximate analytical models and full descriptions by means of Monte Carlo simulations. (Author)

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

    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.

  13. Study of analytical sensitivity of two portable X-ray Fluorescence systems for archaeological obsidians analysis

    The study of archaeological and cultural heritage artifacts by means of analytical techniques with portable equipment has become increasingly routinely today. Various types of portable EDXRF equipment have been used in many different situations involving in situ analysis covering a wide range of geometries, detectors, current and voltage applied in the X-ray tubes. Therefore, it is extremely important that the geometry of the portable systems used in these studies be suitable for accurate acquisition and subsequent analysis of data. This work aim to improve the analytical sensitivity for elemental determination in archaeological objects in the laboratory and in situ, especially obsidian. The measurements were performed with two portable Energy Dispersion X-ray Fluorescence (EDXRF) systems. The variables studied were: distance between sample and detector, distance between sample and X-ray tube, current applied in X-ray tube and voltage applied in X-ray tube. The PXRF-LFNA-02 system, used for analysis of elements with atomic number greater than 26, is composed of a 4W X-ray tube (with Ag filter and target) and a Si-PIN detector model XR-100CR Ampetc Inc., which has a resolution of 221eV for the 5.9 keV line (25μm-thickness Be window and Ag collimator). For the analysis of elements with atomic number lower than 26 the system used was PXRF-LFNA-03, composed of a 4W X-ray tube with W target and a Si-PIN detector, model XR - 100CR of Ampetc Inc., which has a resolution of 149eV for the 5.9 keV line (12.7μm-thickness Be window and Ag collimator). The results showed that the best values for the investigated variables, which resulted in better analytical sensitivity for the two systems were: for PXRF-LFNA-02, Current 8μA and Voltage 35kV, distance between sample and tube 1.4cm, distance between sample and detector 1.7 cm, and for PXRF-LFNA-03, Current 3μA and Voltage 30kV, distance between sample and tube 1.9 cm, distance between sample and detector 2.3 cm. (author)

  14. Energy dispersive X-ray fluorescence analysis of marine pollution indicators

    A methodology for the application of EDXRF with a X-ray tube, in the analysis of elements is shown in the following matrices: microalgae, marine algae, marine sediments and corals. Various methods were applied: one using a relative external standard, a fundamental parameters method, an absolute method based on elemental sensitivity, a method which used X-ray fluorescence excitation measured in the back side of the sample for low contents heavy elements determination and a TRXRF method. The thin layer samples were prepared using a plastic resin. The analyzed samples of marine algae, marine sediments and corals belong to a marine ecosystem from the North of Havana City, the most affected area by natural metereological phenomena and human impact. (author)

  15. The studies of post-medieval glass by multivariate and X-ray fluorescence analysis

    Multivariate statistical analysis of the results obtained by energy dispersive X-ray fluorescence analysis has been used in the study of baroque vessel glasses originated from central Europe. X-ray spectrometry can be applied as a completely non-destructive, non-sampling and multi-element method. It is very useful in the studies of valuable historical artefacts. For the last years, multivariate statistical analysis has been developed as an important tool for the archaeometric purposes. Cluster, principal component and discriminant analysis were applied for the classification of the examined objects. The obtained results show that these statistical tools are very useful and complementary in the studies of historical objects. (author)

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

    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. (paper)

  17. Radiography imaging of cultural heritage obtained with a modified portable X-Ray Fluorescence System

    The sufficiency of imaging quality of the radiographies obtained with a modified portable X-ray fluorescence spectrometer was evaluated for the study of cultural heritage. The proposed instrument use an X-ray tube with Pd anode (2 mm) that allows a maximum voltage and current of 50 kV and 1 mA respectively and a collimation system permit to irradiate a square shape region in the analyzed object by the projection of light beam with the same shape on its surface. The spatial resolution of the obtained radiographic image make possible to localize and well define pentimenti in painting, identify filling materials in a painting under restoration process, the radiogrametry of archaeological bone and the identification of a petrified sphere from an archaeological discovery. The radiographic analysis is proposed for study of physical anthropology in Cuba. (author)

  18. Synchrotron X-ray diffraction and fluorescence study of the astrolabe

    The astrolabe is an ancient analogue astronomical computing device used for calculations relating to position and time of the observer's location. In its most common form (the planispheric astrolabe), it consists of an engraved plate or series of plates held together and pinned in a housing, the assembly usually being made of brass. The present study describes the use of X-ray diffraction (XRD) and X-ray fluorescence (XRF) in a synchrotron to elucidate the composition of, and fabrication techniques used for, the major component parts of the astrolabe. The synchrotron XRF studies are compared to similar studies made with a handheld XRF instrument and the advantages and disadvantages of both approaches are discussed. (orig.)

  19. A multi-channel monolithic Ge detector system for fluorescence x-ray absorption spectroscopy

    Construction and performance of a monolithic quad-pixel Ge detector for fluorescence x-ray absorption spectroscopy (XAS) at synchrotron radiation sources are described. The detector semiconductor element has an active surface area of 4.0 cm2 which is electrically separated into four 1.0 cm2 pixels, with little interfacial dead volume. Spatial response of the array shows that cross-talk between adjacent pixels is 55Fe test source (MnKα, 5.9 keV), energy resolution of better than 200 eV is achieved with a 4 μsec peaking time. At 0.5 μsec peaking time, pulse pileup results in a 75% throughput efficiency for an incoming count rate of 100 kHz. Initial XAS fluoresncece measurements at the beamline 4 wiggler end stations at SSRL show that the detector system has several advantages over commercial x-ray spectrometers for low-concentration counting

  20. Uranium determination at ppb levels by X-ray fluorescence after its preconcentration on polyurethane foam

    A sensitive method based on the preconcentration of uranium on powdered polyurethane foam (PUF) has been developed to determinate this element in water samples by X-ray florescence. Uranium at ppb levels was sorbed as the salicylate complex on powdered PUF at pH 4.0. The resulting PUF was filtered through a filter paper and used for X-ray fluorescence measurements. For 50 μg/l of uranium the coefficient of variation for five measurements is 5% and the detection limit is 5.5 μg/l. The interference level of various ions and ligands was studied and optimum conditions were developed to determine uranium in reference materials, waste water, mine drainage, and sea water. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

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

    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.

  2. Energy dispersive x-ray fluorescence analysis of latin-american pottery

    Energy Dispersive X-Ray Fluorescence Analysis (EDXRF) induced by low power X- Ray tubes provides relatively inexpensive, fast and quantitative method of analysis with good reproducibility and sensitivity, in the field of archaeometry in general and for the analysis of ceramics in particular. Ancient Latin-American potteries have been analyzed: tupiguarani Brazilian pottery from the Fazenda Sta Dalmacia, Cambe', city; Mayan pottery from the Yucatan, Mexico, tainos cuban pottery, from Baracoa region. Minor and trace elements have been identified, that can be classified into three groups, following their atomic number and the EDXRF excitation energy: elements with low atomic number, such as K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn; elements with medium atomic number such as Rb, Sr, Y, and Zr; and Ba

  3. Application of X-ray fluorescence (WDXRF): thickness and chemical composition determination of thin films

    In this work a procedure is described for thickness and quantitative chemical composition of thin films by wavelength dispersion X-ray fluorescence (WDXRF) using Fundamental Parameters method. This method was validated according to quality assurance standard and applied sample Al, Cr, TiO2, Ni, ZrO2 (single thickness) and Ni/Cr (double thickness) on glass; Ni on steel and metallic zinc and TiO2 on metallic iron (single thickness), all the sample were prepared for physical deposition of vapor (PVD). The thickness had been compared with Absorption (FRX-A) and Rutherford Backscattering Spectrometry (RBS) methods; the result showed good efficiency of the fundamental parameters method. Sample structural characteristics analyzed by X ray diffraction (XRD) showed any influence in the thickness determinations. (author)

  4. Synchrotron X-ray diffraction and fluorescence study of the astrolabe

    Notis, Michael [Lehigh University, Bethlehem, PA (United States); Newbury, Brian [ExxonMobil Development Company, Houston, TX (United States); Stephenson, Bruce [Adler Planetarium and Astronomy Museum, Chicago, IL (United States); Stephenson, G.B. [Argonne National Laboratory, Argonne, IL (United States)

    2013-04-15

    The astrolabe is an ancient analogue astronomical computing device used for calculations relating to position and time of the observer's location. In its most common form (the planispheric astrolabe), it consists of an engraved plate or series of plates held together and pinned in a housing, the assembly usually being made of brass. The present study describes the use of X-ray diffraction (XRD) and X-ray fluorescence (XRF) in a synchrotron to elucidate the composition of, and fabrication techniques used for, the major component parts of the astrolabe. The synchrotron XRF studies are compared to similar studies made with a handheld XRF instrument and the advantages and disadvantages of both approaches are discussed. (orig.)

  5. X-ray fluorescence as a tool for investigating archaeological finds

    X-ray fluorescence analysis (XRFA) is an outstanding method for investigations of various objects of historic and cultural significance, as it is non-destructive, can be used without any sampling of the analysed artefacts and, if necessary, measurements can be carried out in situ. The laboratory at CTU FNSPE is equipped for XRFA with radionuclides 55Fe, 238Pu and 241Am and with a small X-ray tube (30 kV) as excitation sources, and with Si(Li) and Si-PIN semiconductor spectrometers for detecting XRF spectra. This paper deals with XRFA of archaeological finds. Practical examples are selected from investigations of ceramic objects from excavations in the Czech Republic

  6. X-ray fluorescence as a tool for investigating archaeological finds

    Cechak, T. [Department of Dosimetry and Application of Ionising Radiation, Czech Technical University in Prague, Faculty of Nuclear Sciences and Physical Engineering, Brehova 7, 115 19 Prague 1 (Czech Republic); Hlozek, M. [Department of Archaeology and Museology, Masaryk University, Faculty of Arts, Arna Novaka 1, 602 00 Brno (Czech Republic)], E-mail: musilek@fjfi.cvut.cz; Musilek, L.; Trojek, T. [Department of Dosimetry and Application of Ionising Radiation, Czech Technical University in Prague, Faculty of Nuclear Sciences and Physical Engineering, Brehova 7, 115 19 Prague 1 (Czech Republic)

    2007-09-21

    X-ray fluorescence analysis (XRFA) is an outstanding method for investigations of various objects of historic and cultural significance, as it is non-destructive, can be used without any sampling of the analysed artefacts and, if necessary, measurements can be carried out in situ. The laboratory at CTU FNSPE is equipped for XRFA with radionuclides {sup 55}Fe, {sup 238}Pu and {sup 241}Am and with a small X-ray tube (30 kV) as excitation sources, and with Si(Li) and Si-PIN semiconductor spectrometers for detecting XRF spectra. This paper deals with XRFA of archaeological finds. Practical examples are selected from investigations of ceramic objects from excavations in the Czech Republic.

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

    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.

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

    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.

  9. Development of a software for reconstruction of X-ray fluorescence intensity maps

    The technique of X-ray fluorescence (XRF) using SR microbeams is a powerful analysis tool for studying elemental composition in several samples. One application of this technique is the analysis done through the mapping of chemical elements forming a matrix of data. The aim of this work is the presentation of the program MapXRF, an in-house software designed to optimize the processing and mapping of fluorescence intensities data. This program uses spectra generated by QXAS as input data and separates the intensities of each chemical element found in the fluorescence spectra in files themselves. From these files, the program generates the intensity maps that can be visualized in any program of treatment of images. The proposed software was tested using fluorescence data obtained in the XRF beamline of XRF at Synchrotron Light National Laboratory (LNLS), Brazil. Automatic 2D scans were performed and element distribution maps were obtained in the form of a matrix of data. (author)

  10. The accuracy of X-ray fluorescence spectrometric determination of Rb and Sr contents in rock sample

    It is shown that application of the Compton scattering method in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide element contents at an accuracy level +- 1 %

  11. Study of the elemental composition of Chenopodium Quinoa Willd by fast neutron activation analysis and X ray fluorescence analysis

    By means of x-ray fluorescence and fast neutron activation analysis the nitrogen content has been determined in samples of roots, stems, leaf, flowers and grains from Quinua (Chenopodium Quinoa Willd), which was previously treated with fertilizer

  12. Non-destructive plant-nutrition analysis by neutron analysis by neutron activation and X-ray fluorescence techniques

    Non-destructive neutron activation and x-ray fluorescence techniques have been applied to the analysis of plant nutrients in soil. The advantages of these methods over the conventional ones have also been focussed. (author)

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

    Das, Gangadhar; Kane, S. R.; Khooha, Ajay; Singh, A. K.; Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in [Indus Synchrotrons Utilization Division, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India)

    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.

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

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

    2015-05-01

    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. PMID:26026553

  15. Quantitative analysis of soil by using X-ray fluorescence spectrometry (WDXRFS)

    Development of the new technologies has been using a lot of substances composed by metals, consequently generating reject for the environment. There is nowadays a concern in management and to control processes that contribute to the environmental degradation. This paper has the purpose to establish an analysis method for the quantitative determination of major and trace elements soil used the Technique of Wavelength Dispersion X-ray Fluorescence Spectrometry (WDRXFS) and the Fundamental Parameters Method. This method allows calculating the theoretical fluorescent intensities obtained by the measured intensities of the elements present in the sample, through the instrumental sensibility. Advantages of this methodology are: use of small amount of sample, accuracy high and sensibility in the determinations studied analyte; not use of chemical treatments in the preparation of samples; speed and cost relatively low. Methodology was validated by the analyze of five certified reference materials, CRM-2704 - Buffalo River Sediment (NIST), JB2, JG1 and JG1a - Geological Survey of Japan (GSJ) and SL-3 -Lake Sediment (IAEA). An X- Ray Fluorescence Spectrometer RIGAKU was used, RIX 3000, 1996 of the Laboratory X-Ray Fluorescence, Center of Chemistry and environment of the Institute of Energy and Nuclear Researches of Sao Paulo. The detection limit for major elements is 0,01-0,2% and trace elements 5 μg/g-100 μg/g. The analytes studied were: SiO2, TiO2, Al2O3, Fe2O3, MnO, MgO, CaO, Na2O, K2O, P2O5, Ag, As, Cd, Ce, Cr, Cu, Ga, Hg, La, Nd, Ni, Pb, Rb, Se, Sr, V, Y, Zn and Zr. (author)

  16. Technique of sample preparation for analysis of gasoline and lubricating oils by X-ray fluorescence analysis

    The X-ray fluorescence laboratory of the National Institute of Nuclear Research when not having a technique for the analysis of oils it has intended, with this work, to develop a preparation technique for the analysis of the metals of Pb, Cr, Ni, V and Mo in gasolines and oils, by means of the spectrometry by X-ray fluorescence analysis. The obtained results, its will be of great utility for the one mentioned laboratory. (Author)

  17. Determination of soluble elements in water by x-ray fluorescence spectrometry after preconcentration with polyvinylpyrrolidone-thionalide

    A method for the quantitative determination of soluble elements such as Fe, Cu, Zn, Se, Cd, Sn, Te, Hg, and Pb in water is described. This method is based on preconcentrating the dissolved elements with the combined organic precipitating reagents polyvinylpyrrolidone and thionalide, filtering the precipitate to form a suitable x-ray sample, and analyzing the sample by x-ray fluorescence. Large concentrations of calcium and magnesium do not interfere when the method is applied to natural and waste water samples. X-ray fluorescence analysis can achieve detection limits in the microgram-per-liter range for all elements tested

  18. X-ray fluorescence and computed radiography analysis of a famous brazilian painting from XIX century

    Calza, Cristiane; Oliveira, Davi F.; Rocha, Henrique S.; Lopes, Ricardo Tadeu [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Lab. de Instrumentacao Nuclear], e-mail: ccalza@lin.ufrj.br; Pedreira, Andrea [Museu Nacional de Belas Artes, Rio de Janeiro, RJ (Brazil)

    2009-07-01

    This work used Energy Dispersive X-Ray Fluorescence (EDXRF) and Computed Radiography (CR) to evaluate the general conditions of the painting 'Gioventu' (Eliseu Visconti, 1898), identifying possible problems, areas that revealed signs of previous retouchings and the pigments used by the artist. EDXRF measurements were carried out with a portable system consisting of an X-ray tube Oxford TF3005 with W anode, operating at 25 kV and 100 {mu}A, and a Si-PIN XR-100CR detector from Amptek. Several spectra were obtained in each color, with an acquisition time of 300 s and a beam collimation of 2 mm. The spectra were analyzed using the software QXAS-AXIL (IAEA). The results revealed that the drawings were made over a preparatory layer of lead white. Some pigments identified were: yellow, red and brown ochre; umbra; vermilion; cobalt blue; etc. The experimental setup used in the CR analysis consisted of an Oxford X-ray source, operating at 50 kV and 200 {mu}A, placed at 85 cm from the painting, a GE CR 50P portable computed radiography scanner and a Fuji imaging plate detector. The exposure time was 600 s. The radiographic images revealed that the painting was in a good state of conservation and also a complete composition hidden underneath the visible paint layer.(author)

  19. Integration of X-ray micro tomography and fluorescence for applications on natural building stones

    Dewanckele, J.; Cnudde, V.; Boone, M.; Van Loo, D.; De Witte, Y.; Pieters, K.; Vlassenbroeck, J.; Dierick, M.; Masschaele, B.; Van Hoorebeke, L.; Jacobs, P.

    2009-09-01

    X-ray computed tomography (CT) is an excellent, non-destructive analysis tool for characterising many different materials. In geosciences, 3D visualisation is becoming of prime importance in characterising internal structures of various rock types. It enables new approaches in petrophysical research of rock components, including pore and mineral distribution. Although CT provides a lot of information, this technique is limited concerning information on chemical element distribution. X-ray fluorescence (XRF) on the other hand is an excellent technique to obtain the missing information on chemical properties. At the recently established "Centre for X-ray Tomography" of Ghent University (UGCT) a micro- and nanoCT scanner has been constructed. It is expected that by combination of high-resolution CT and XRF it will be possible to characterise the spatial mineral and element distribution. The combination of both techniques has been applied on natural building stones, in order to get a better insight into some geological parameters (porosity, pore structure, mineral distribution, colour, grain orientation, etc.). Afterwards, the integration of the Morpho+ software tool provides us a 3D quantification of the resulting data.

  20. Integration of X-ray micro tomography and fluorescence for applications on natural building stones

    X-ray computed tomography (CT) is an excellent, non-destructive analysis tool for characterising many different materials. In geosciences, 3D visualisation is becoming of prime importance in characterising internal structures of various rock types. It enables new approaches in petrophysical research of rock components, including pore and mineral distribution. Although CT provides a lot of information, this technique is limited concerning information on chemical element distribution. X-ray fluorescence (XRF) on the other hand is an excellent technique to obtain the missing information on chemical properties. At the recently established 'Centre for X-ray Tomography' of Ghent University (UGCT) a micro- and nanoCT scanner has been constructed. It is expected that by combination of high-resolution CT and XRF it will be possible to characterise the spatial mineral and element distribution. The combination of both techniques has been applied on natural building stones, in order to get a better insight into some geological parameters (porosity, pore structure, mineral distribution, colour, grain orientation, etc.). Afterwards, the integration of the Morpho+ software tool provides us a 3D quantification of the resulting data.

  1. Integration of X-ray micro tomography and fluorescence for applications on natural building stones

    Dewanckele, J; Cnudde, V; Pieters, K; Jacobs, P [Department of Geology and Soil Science, Ghent University, Krijgslaan 281/S8, B-9000 Gent (Belgium); Boone, M; Loo, D Van; De Witte, Y; Vlassenbroeck, J; Dierick, M; Masschaele, B; Hoorebeke, L Van, E-mail: Jan.Dewanckele@UGent.b [Department of Subatomic and Radiation Physics, Ghent University, Proeftuinstraat 86, B-9000 Gent (Belgium)

    2009-09-01

    X-ray computed tomography (CT) is an excellent, non-destructive analysis tool for characterising many different materials. In geosciences, 3D visualisation is becoming of prime importance in characterising internal structures of various rock types. It enables new approaches in petrophysical research of rock components, including pore and mineral distribution. Although CT provides a lot of information, this technique is limited concerning information on chemical element distribution. X-ray fluorescence (XRF) on the other hand is an excellent technique to obtain the missing information on chemical properties. At the recently established 'Centre for X-ray Tomography' of Ghent University (UGCT) a micro- and nanoCT scanner has been constructed. It is expected that by combination of high-resolution CT and XRF it will be possible to characterise the spatial mineral and element distribution. The combination of both techniques has been applied on natural building stones, in order to get a better insight into some geological parameters (porosity, pore structure, mineral distribution, colour, grain orientation, etc.). Afterwards, the integration of the Morpho+ software tool provides us a 3D quantification of the resulting data.

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

    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.

  3. X-ray fluorescence analysis of airborn particulates in an industrial Greek city

    Photon-induced X-ray fluorescence is used at a medium-sized Greek industrial city to detect trace elements with 20(109Cd source which emits mainly Ag X-rays, has been used in a π-geometry. The source in the form of a ring was housed in an aluminium shield backed with iron. In the center of the ring a small hole allowed viewing of the sample by a Si(Li) detector. The latter had a resolution of about 0.18 keV FWHM for the Mn Kα X-ray. The calibration of the system was made by using targets of well known thicknesses. Samples of airborn dust were collected by drawing with a pump about 10 m3 of air through a Whatman 41 filter paper. The volume of the air passed was measured with a gas meter. Efficiency of the air filtration was estimated by using two filters in series during air sampling. The efficiency of collection for each element was then estimated from the measured amount of each element at the two filters. Tabulated data are given. (T.G.)

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

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

  5. Methodology for determination of inorganic elements in vitamin supplements by X-ray fluorescence

    A methodology is present for qualification of inorganic elements in alimentary supplements, using a portable system of low power X-ray, in the analysis of two commercial products, both found as pills. The PXRF (Portable X-ray Fluorescence) is a X-ray mini tube, Ag filter at tube exit, a Si-Pin semiconductor and a Ag collimator at the detector entry, specific circuitry for this type of system and a microcomputer for the data acquisition and analysis. Samples and standards were diluted in boric acid, and the samples were prepared in a 1:10 rate, and the standards vary of 1:2, 1;5, 1:10. 1:15 and 1:100. Results were obtained for Ca, Ti, Mn, Fe, Cu e Zn, with values varying from 0.14 to 8.45 for the sample A, and from 0.17 to 17.94 for the sample B. The PXRF portable system demonstrated to be a multi elementary analysis tool with high analytical speed, and can be applied in situ no only for quality control but also for monitoring of inspection organism

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

    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.

  7. X-ray fluorescence and computed radiography analysis of a famous brazilian painting from XIX century

    This work used Energy Dispersive X-Ray Fluorescence (EDXRF) and Computed Radiography (CR) to evaluate the general conditions of the painting 'Gioventu' (Eliseu Visconti, 1898), identifying possible problems, areas that revealed signs of previous retouchings and the pigments used by the artist. EDXRF measurements were carried out with a portable system consisting of an X-ray tube Oxford TF3005 with W anode, operating at 25 kV and 100 μA, and a Si-PIN XR-100CR detector from Amptek. Several spectra were obtained in each color, with an acquisition time of 300 s and a beam collimation of 2 mm. The spectra were analyzed using the software QXAS-AXIL (IAEA). The results revealed that the drawings were made over a preparatory layer of lead white. Some pigments identified were: yellow, red and brown ochre; umbra; vermilion; cobalt blue; etc. The experimental setup used in the CR analysis consisted of an Oxford X-ray source, operating at 50 kV and 200 μA, placed at 85 cm from the painting, a GE CR 50P portable computed radiography scanner and a Fuji imaging plate detector. The exposure time was 600 s. The radiographic images revealed that the painting was in a good state of conservation and also a complete composition hidden underneath the visible paint layer.(author)

  8. Sample preparation of waste water to determine metallic contaminants by X-ray fluorescence spectroscopy

    Trace X-ray fluorescence spectroscopy analysis in liquid samples is preceded by sample preparation, which usually consists in the precipitation of the metallic ions and concentration over a thin cellulose filter. The samples preparation of waste water by this method is not efficient, due to the great amount of organic and insoluble matter that they contain. The purpose of this work was to determine the optimal value of pH in order to adsorbe all the insoluble matter contained in a waste water sample in the activated charcoal, so that the metallic ions could be precipitated and concentrated on a thin filter and determinated by X-ray fluorescence spectroscopy. A survey about the adsorption of some ions in activated charcoal in function of the pH was made for the following: Cr3+, Fe3+, Ni2+, Cu2+, Zn2+, Se2+, Hg2+, and Pb2+. It was observed that at pH 0, the ions are not adsorbed, but Cu2+ and Zn2+ are adsorbed in small amount; at pH 14, the ions are adsorbed, excluding Se, which is not adsorbed at any value of pH. If a waste water sample is treated at pH 0 with activated charcoal to adsorbe the organic and insoluble matter, most of the metallic ions are not adsorbed by the activated charcoal and could be precipitated with APDC (ammonium 1-pirrolidine dithio carbamate salt) and concentrated on a thin filter. The analysis of the metallic ions contained on the filter and those adsorbed in the activated charcoal by X-ray fluorescence spectroscopy, gave the total amount of the ions in the sample. (author)

  9. Application of X-ray fluorescence method for elemental analysis of PM2.5 fraction

    Samek Lucyna

    2015-09-01

    Full Text Available The scientific interest in air pollution comes from its influence on human health, the condition of cultural heritage and climate. The PM2.5 fraction (particles of a diameter of 2.5 mm or below, indirectly, has a significant impact on health which is associated with respiratory tract and blood vessel related diseases. However, not only the size, but also the content of the particles has a significant meaning. To determine the particulate matter contents, elemental analysis can be performed using numerous techniques, the most important of which is X-ray fluorescence. In this study, samples of PM2.5 fraction collected in Krakow, Poland were analyzed. The X-ray fluorescence method was used to perform elemental analysis. The gravimetric method was applied to determine the concentration of the PM2.5 fraction. Low detection limits of individual elements and precision of the X-ray fluorescence method were determined. The concentrations of the following elements: Cl, K, Ca, Cr, Mn, Fe, Cu, Zn, Br, Rb, Sr and Pb in the PM2.5 fraction samples collected in Krakow were evaluated. The homogeneity of the samples was also estimated. The concentrations of PM2.5 fraction collected in the summer of 2013 were in the range of 6-23 ng/m3. The concentrations of PM2.5 fraction collected in the winter of 2013 were in the range of 26-171 ng/m3. The precision of the method was found to be below 1% for elements with high concentration in the sample and 6-8 % for trace elements.

  10. [Establishment and Improvement of Portable X-Ray Fluorescence Spectrometer Detection Model Based on Wavelet Transform].

    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. PMID:26197612

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

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

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

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

    2008-12-15

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

  13. Maia X-ray fluorescence imaging: Capturing detail in complex natural samples

    Ryan, C. G.; Siddons, D. P.; Kirkham, R.; Li, Z. Y.; de Jonge, M. D.; Paterson, D. J.; Kuczewski, A.; Howard, D. L.; Dunn, P. A.; Falkenberg, G.; Boesenberg, U.; De Geronimo, G.; Fisher, L. A.; Halfpenny, A.; Lintern, M. J.; Lombi, E.; Dyl, K. A.; Jensen, M.; Moorhead, G. F.; Cleverley, J. S.; Hough, R. M.; Godel, B.; Barnes, S. J.; James, S. A.; Spiers, K. M.; Alfeld, M.; Wellenreuther, G.; Vukmanovic, Z.; Borg, S.

    2014-04-01

    Motivated by the challenge of capturing complex hierarchical chemical detail in natural material from a wide range of applications, the Maia detector array and integrated realtime processor have been developed to acquire X-ray fluorescence images using X-ray Fluorescence Microscopy (XFM). Maia has been deployed initially at the XFM beamline at the Australian Synchrotron and more recently, demonstrating improvements in energy resolution, at the P06 beamline at Petra III in Germany. Maia captures fine detail in element images beyond 100 M pixels. It combines a large solid-angle annular energy-dispersive 384 detector array, stage encoder and flux counter inputs and dedicated FPGA-based real-time event processor with embedded spectral deconvolution. This enables high definition imaging and enhanced trace element sensitivity to capture complex trace element textures and place them in a detailed spatial context. Maia hardware and software methods provide per pixel correction for dwell, beam flux variation, dead-time and pileup, as well as off-line parallel processing for enhanced throughput. Methods have been developed for real-time display of deconvoluted SXRF element images, depth mapping of rare particles and the acquisition of 3D datasets for fluorescence tomography and XANES imaging using a spectral deconvolution method that tracks beam energy variation.

  14. A high resolution x-ray fluorescence spectrometer for near edge absorption studies

    A high resolution fluorescence spectrometer using a Johann geometry in a back scattering arrangement was developed. The spectrometer, with a resolution of 0.3 eV at 6.5 keV, combined with an incident beam, with a resolution of 0.7 eV, form the basis of a high resolution instrument for measuring x-ray absorption spectra. The advantages of the instrument are illustrated with the near edge absorption spectrum of dysprosium nitrate. 10 refs., 4 figs

  15. Qualitative and quantitative analysis of medieval silver coins by energy dispersive X-ray fluorescence method

    Energy-dispersive X-ray fluorescence spectrometry was applied for the analysis of historical silver coins to determine the elemental composition in a fast and non-destructive way. Ag, Cu and trace elements (V, Cr, Mn, Fe, Co, Ni, Hg, Pd, Zr, Mo, Rh, Ru) were determined in coins of King Mathias (Hungary, 1458-1490). A new data evaluation technique was used to avoid the problems arising from the different sizes, surfaces and geometries. The appropriateness of this method was confirmed by analysing certified silver/copper standard alloys. (author)

  16. An x-ray fluorescence study of lake sediments from ancient Turkey using synchrotron radiation.

    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.

  17. Chemical characterization of clay SRM by X-ray fluorescence – results comparison from different laboratories

    Carlos Roberto Appoloni

    2009-03-01

    Full Text Available Two Energy Dispersive X-ray Fluorescence equipments have been compared in order to verify its performance for clay characterization and potential application to the study in archaeometric field and industry. Two clay standard reference materials (SRM, IPT-42 and IPT-51 and one IAEA intercomparison sample were analyzed by two different methodologies and equipments. Asentamiento Universitario Zapala laboratory has a Shimadzu EDX-800HS bench top equipment and 13 elements from S to Zr were quantified in the standards. Applied Nuclear Physics Laboratory has a portable EDXRF system. It was possible to quantify K, Ti and Fe and qualitatively to identify Mn, Rb, Zn and Zr.

  18. Thorium determination by X-ray Fluorescence Spectrometry in simulated thorex process solutions

    The X-ray fluorescence method for thorium determination in aqueous and organic (TBP-n-dodecane) solutions is described. The thin film-technique for sample preparation and a suitable internal standard have been used. Some parameters as analytical line, internal standard, filter paper, paper geometry, sample volume and measurement conditions were studied. Uranium, fission products, corrosion products and thorex reagent components were studied as interfering elements in the thorium analysis, as well as the matrix effect by using the thorex process simulated solutions the method to thorium determination in irradiated thorium solutions was applied. (M.J.C.)

  19. Separation of substandard tin ores by x-ray fluorescence method

    Analysis of pure tin ores on X-ray fluorescence separation (XFS) is carried out. The volumes of lump sampling are substantiated; several variants of technical and economical efficiency of XFS application have been calculated. It is shown that at XFS of -400+25 mm classes conditional as to tin content intermediate product with high efficiency factor may be prepared. Separation of -25+10 mm class is unsuitable, as it doesn't allow to increase tin content to conditional, and the process efficiency is low

  20. X-ray fluorescence analysis of obsidian objects from Catamarca, Argentina

    The concentrations of five trace elements (Rb, Zr, Sr, Ti and Mn) and one major (Fe) element have been determined in groups of obsidian samples by wavelength dispersive X-ray fluorescence spectrometry. Two methods were used for different elements on the basis of different excitation conditions and sample preparation procedures. Synthetic standards with compositions similar to those of the igneous stone were prepared into which the analytes were incorporated in solution. The method was used to establish the provenance of a number of prehistoric obsidian artifacts. The results ascertained in these analyses are discussed in this paper. (author) 16 refs.; 1 fig.; 3 tabs

  1. The x-rays fluorescence applied to the analysis of alloys

    This work is based on the utilization of the Fluorescence of X Rays. This technique of non destructive trial, has the purpose to establish a routine method, for the control of the conformation of industrial samples used. It makes an analysis with a combination of the algorithms of Rasberry-Heinrich and Claisse-Thinh. Besides, the numerical implementation of non usual techniques in this type of analysis. Such as the Linear Programming applied to the solution of super determined systems, of equations and the utilization of methods of relaxation to facilitate the convergence to the solutions. (author)

  2. Analysis of refractories by the method of X-ray fluorescence

    The results of the analysis by the method of X-ray fluorescence spectrometry in refratories, comparing the behavior of samples prepared using sodium tetraborate and lithium tetraborate as flux in pellets preparation, are discussed. It is concluded that the utilization of lithium tetraborate gives more resistance to the superficial deterioration of pellets and better analitic sensitivity. No significant differences in reproducibility are shown provided that the care required in the handle of sodium tetraborate pellets is observed. The utilization of lithium tetraborate pellets is recomended, because of the simplification that they bring to the routine operation, as a consequence of the greater estability of their surface conditions. (E.G.)

  3. Fast neutron activation analysis and radioisotope X-ray fluorescence study on KALEWA and NAMMA coal

    Kalewa coal was studied with Fast Neutron Activation Analysis (FNAA) technique, employing KAMAN A-710 neutron generator and HP(Ge) detector coupled to ''Canberra'' series 30 MCA. Sequential irradiation and dual aluminium foil monitoring method was employed. Simultaneous multielement analysis was carried out. Namma Coal was studied with radioisotope X-ray Fluorescence (XRF) technique, employing Co-57 exciter source and HP(Ge) detector coupled to ''Canberra'' series 40 MCA. In both FNAA and XRF study, the results obtained were compared to that obtained with Atomic Absorption Spectrophotometry (AAS) technique. Finally, the results were reviewed together with those obtained from similar work on coal with FNAA and XRF techniques. (author)

  4. Determination of copper in the environment by X-ray fluorescence method

    The effective rapid X-ray fluorescence method for determination of copper in atmospheric air, soil, food, plants, and biological media is developed. Sup(238)Pu radionuclide, RPSCh-01 device, S1-6R proportional counter or scintillator detector with NaI(Tl) crystal were used during the analyses. Methods of preparation of samples for analysis are described in short. Calculation was performed using calibration curve. This method is widely tested in sanitary investigations in the region of large copper-sulphur integrated industrial plant. Sensitivity of determination is 0.05 μg, analysis accuracy is 3-5%

  5. The determination of nanogram amounts of Chromium in urine by x-ray fluorescence spectroscopy

    Beyermann, K.; Rose, H.J., Jr.; 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.

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

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

    2014-04-24

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

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

    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

  8. In-Situ Silver Acetylide Silver Nitrate Explosive Deposition Measurements Using X-Ray Fluorescence.

    Covert, Timothy T.

    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.

  9. Pattern recognition on X-ray fluorescence records from Copenhagen lake sediments using principal component analysis

    Schreiber, Norman; Garcia, Emanuel; Kroon, Aart;

    2014-01-01

    Principle Component Analysis (PCA) was performed on chemical data of two sediment cores from an urban fresh-water lake in Copenhagen, Denmark. X-ray fluorescence (XRF) core scanning provided the underlying datasets on 13 variables (Si, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Rb, Cd, Pb). Principle...... depths. The sediments featured a temporal association with contaminant dominance. Lead contamination was superseded by zinc within the compound pattern which was linked to changing contamination sources over time. Principle Component Analysis was useful to visualize and interpret geochemical XRF data...

  10. The determination, by x-ray-fluorescence spectrometry, of gold in activated charcoal

    A rapid method is described for the determination of gold in activated charcoal by X-ray-fluorescence spectrometry. Compensation for matrix effects is achieved by means of platinum that is added for use as an internal standard. Calibration is achieved by use of a series of synthetic standards that are made by the spiking of barren charcoal with gold and platinum. The limit of determination is about 8 p.p.m. of gold, and the relative standard deviation is 1,2 per cent at a concentration level of 2300 p.p.m

  11. Analysis of Jamaican soils and sediments by energy-dispersive X-ray fluorescence spectrometry

    The calibration of a tube excited Energy-Dispersive X-Ray Fluorescence spectrometer for routine geochemical analyses of Ca, Ti, V, Cr, Mn, Fe, Cu, Zn, Rb, Sr and Pb in Jamaican soils and sediments is described. Simple linear and parabolic regression models using scattered radiation and an element as internal standards were applied. The analysis of over 200 samples from a regional soil survey has been used to contribute to a database on the geochemistry of Jamaican soils and sediments. An application example of the Zn distribution map in Jamaican soils is presented. (author). 20 refs., 5 figs., 4 tabs

  12. Clinical applications of total reflection X-Ray Fluorescence in the treatment of cancer, Preliminary results

    A simple procedure is presents in which direct irradiation of small (10 ?l) quantities of blood serum, without chemical treatment or internal standard addition, allows reliable quantification of the PT plasma level with a 300 ppb detection limit and precision of 7% (n=7) It is shown that the method allows determination of the time evolution of the drug concentration and the drug half life in the patient the results indicated the viability of an improvement in the clinical practice of chemotherapy by the routine analysis of platinum with total reflection X-Ray Fluorescence

  13. The design of X-ray fluorescence analyzer based on Labview and USB technique

    The new X-ray fluorescence analyzer is presented. The design of multi-channel nuclear spectrum analyzer, based on ADμC812, was introduced in details, and as well as application program design based on Labview, and how to write the USB of drive procedure was given also. It can analyze the output of the radiation detector by multi-channel nuclear spectrum analyzer and give the height spectrum by USB interface. The results indicate that the system has the characteristics of perfect function, reliable performance. (authors)

  14. Selection of polychlorinated plastics in plastic waste by X-ray fluorescence method

    The X-ray fluorescence method using a small source of 55Fe was examined and found to be applicable for the selection of polychlorinated plastics from plastic waste in model areas in Tokyo designated for investigating their content in the waste. The weight ratios of soft and hard polychlorinated plastics to the total plastic waste estimated by this method were found to be 15.6% and 0.29% respectively. These values agree well with the results obtained with the Beilstein method. (author)

  15. On-line X-ray fluorescence detection for capillary electrophoresis separations

    In these investigations, capillary electrophoresis with on-line X-ray fluorescence detection (CE-XRF) has been demonstrated for the first time. The insertion of a polyethylene sample cell between fused-silica capillary segments enabled continuous XRF detection during electrophoresis with minimal additional band broadening. Detection limits in the 10-4 M range are currently feasible for the CE-XRF separation of metal complexes, and design advances will enhance detectability to the 10-5-10-6 M range, permitting studies of important environmental and biological samples

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

    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.

  17. Application of data fusion in-situ X-ray fluorescence analysis

    In this paper, effects of surface smoothness, moisture content, density and mineral granularity of the samples on X-ray fluorescence yield are analyzed, and principals of data fusion and modular neural network are introduced. A neural network data fusion model was established, with its learning algorithm for correcting the interfering factors. With the model, error caused by surface smoothness, moisture content and density could be reduced to less than 10%. The results prove that the mathematic models have high precision and the fusion technology of information can be used for in-situ correction of XRF analysis results. (authors)

  18. Heavy metals analysis in blood by the X-ray fluorescence method

    The analytical procedure for determination of heavy metals in blood is described. Blood was taken from active smelter workers, samples were stored in special flasks at 2 grades C. After freeze drying, dried samples was analyzed using X-ray fluorescence, sources excited: Pu-238 and Cd-109 was used. Br in Pb interferences were corrected. The agreement of the results with values in similar workers is satisfactory Median Pb level was 42.6 micro grams/100 ml (total blood), Cu was less 2.5 micro grams/g (dry blood) and Zn was 11 micro grams/g (dry blood). (author)

  19. Investigation of trace elements in hair of athletes by synchrotron radiation X-ray fluorescence analysis

    Trace elements Fe, Zn and Ca in hair samples taken from four athletes have been determined by using SR X-ray fluorescence analysis technique. Each sample is scanned point by point at 1.5 mm of interval, which corresponds to 5 days of hair growth. Preliminary results show that the change of iron content in hair is related to exercise capacity of athletes, but no observable change is found for Zn and Ca content. It is verified that sport is one of the causes leading to iron deficiency of athletes

  20. Analysis of the Peiting Woman Using Portable X-Ray Fluorescence Spectroscopy

    Bauerochse, Andreas

    2013-04-01

    Full Text Available Portable X-ray Fluorescence Spectroscopy was applied to the skeletal remains of 13 bog bodies and their bog burial environments. The objective was to create a better understanding of Northern European bog environmental chemistry and its diagenetic effects on interred bog bodies, determine bog body geographic disparity and/or origin, and identify if post-discovery preservation procedures were applied to the bog body remains. This paper summarizes the findings for one of those 13 bog bodies: the Peiting Woman from Bavaria, Germany. The elements analyzed include Antimony, Cobalt, Copper, Iron, Manganese, Molybdenum, Lead, Strontium, Titanium, Zinc, and Zirconium.

  1. Determination of low concentrations of uranium in granite samples by X-ray fluorescence

    An x-ray fluorescence method for the determination of uranium in granite samples for concentrations ranging from 3 to 100 ppm U3O8 has been developed. To this purpose a sample holder, specially designed, allowing the irradiation of sample surfaces 42.5 mm in diameter and a molybdenum tube operating with a power of 2700 W (90 kV, 30 mA) are used. The background influence and the spectral interferences from rubidium and strontium have been taken into account and specific correction coefficients have been computed. A Basic program facilitates the report of the analytical results. (author)

  2. Soil ratio evaluation in industrial sugar cane by energy dispersive x-ray fluorescence analysis

    The radioisotope induced energy dispersive X-ray fluorescence analysis has been used for the determination of total contents of Al, Si, Ti, Fe, and Zr, chosen as soil tracers in sugar cane consignments. These elements have been evaluated in ten different types of soils from the sugar cane growing area of the sate of Sao Paulo, aiming to establish elemental ratios which could helping the identification and quantification of the soil loaded with the stalks in the field during harvesting of sugar cane. (author). 16 refs, 9 figs, 1 tab

  3. Cardiac output determination during intravenous cardioangiography using X-ray fluorescence analysis

    Boijsen, M.; Goss, F.; Jacobsson, L.; Lamm, C.; Schlossmann, D.; Bjoerneld, L.; Tylen, U.

    Cardiac output was determined with an indicator dilution technique during digital venous angiography of the left ventricle in 11 patients. The contrast medium injected into the right atrium was used as indicator. During and after the injection of contrast medium one blood sample per second was obtained through a catheter placed in the descending aorta. The samples were analyzed for iodine content with X-ray fluorescence analysis and cardiac output determined ad modum Stewart-Hamilton. Thermodilution was used as a reference method. The results indicate that the indicator dilution method with the use of contrast medium might be used for calibration of videodensitometric methods for blood flow measurements.

  4. Corrections for matrix effects in X-ray fluorescence analysis-A tutorial

    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

  5. Elimination of matrix effect in quantitative analysis of elements using x-ray fluorescence

    The emission-transmission method of Leroux and Mahmud, an experimental technique for compensating matrix effects in photon excited X-ray fluorescence analysis, was used to determine the concentration of lead and antimony in pellets of galalith. The effect of interfering elements was studied by adding various concentrations of mercury and tin to the respective pellets. To illustrate possible environmental applications, a number of pellets was prepared from leaves of almond trees located in different regions of Rio de Janeiro. Lead concentrations were determined for the dried leaf material and showed values ranging from 50 to 145 parts per million

  6. X-ray fluorescence imaging system for fast mapping of pigment distributions in cultural heritage paintings

    Conventional X-ray fluorescence imaging technique uses a focused X-ray beam to scan through the sample and an X-ray detector with high energy resolution but no spatial resolution. The spatial resolution of the image is then determined by the size of the exciting beam, which can be obtained either from a synchrotron source or from an X-ray tube with a micro-capillary lens. Such a technique based on a pixel-by-pixel measurement is very slow and not suitable for imaging large area samples. The goal of this work is to develop a system capable of simultaneous imaging of large area samples by using a wide field uniform excitation X-ray beam and a position sensitive and energy dispersive detector. The development is driven by possible application of such a system to imaging of distributions of hidden pigments containing specific elements in cultural heritage paintings, which is of great interest for the cultural heritage research. The fluorescence radiation from the area of 10 × 10 cm2 is projected through a pinhole camera on the Gas Electron Multiplier detector of the same area. The detector is equipped with two sets of orthogonal readout strips. The strips are read out by the GEMROC Application Specific Integrated Circuits (ASIC)s, which deliver time and amplitude information for each hit. This ASIC architecture combined with a Field Programmable Gate Array (FPGA) based readout system allows us to reconstruct the position and the total energy of each detected photon for high count rates up to 5 × 106 cps. Energy resolution better than 20% FWHM for the 5.9 keV line and spatial resolution of 1 mm FWHM have been achieved for the prototype system. Although the energy resolution of the Gas Electron Multiplier (GEM) detector is, by principle, not competitive with that of specialised high energy resolution semiconductor detectors, it is sufficient for a number of applications. Compared to conventional micro-XRF techniques the developed system allows shortening of the

  7. X-ray fluorescence imaging system for fast mapping of pigment distributions in cultural heritage paintings

    Zielińska, A.; Dąbrowski, W.; Fiutowski, T.; Mindur, B.; Wiącek, P.; Wróbel, P.

    2013-10-01

    Conventional X-ray fluorescence imaging technique uses a focused X-ray beam to scan through the sample and an X-ray detector with high energy resolution but no spatial resolution. The spatial resolution of the image is then determined by the size of the exciting beam, which can be obtained either from a synchrotron source or from an X-ray tube with a micro-capillary lens. Such a technique based on a pixel-by-pixel measurement is very slow and not suitable for imaging large area samples. The goal of this work is to develop a system capable of simultaneous imaging of large area samples by using a wide field uniform excitation X-ray beam and a position sensitive and energy dispersive detector. The development is driven by possible application of such a system to imaging of distributions of hidden pigments containing specific elements in cultural heritage paintings, which is of great interest for the cultural heritage research. The fluorescence radiation from the area of 10 × 10 cm2 is projected through a pinhole camera on the Gas Electron Multiplier detector of the same area. The detector is equipped with two sets of orthogonal readout strips. The strips are read out by the GEMROC Application Specific Integrated Circuits (ASIC)s, which deliver time and amplitude information for each hit. This ASIC architecture combined with a Field Programmable Gate Array (FPGA) based readout system allows us to reconstruct the position and the total energy of each detected photon for high count rates up to 5 × 106 cps. Energy resolution better than 20% FWHM for the 5.9 keV line and spatial resolution of 1 mm FWHM have been achieved for the prototype system. Although the energy resolution of the Gas Electron Multiplier (GEM) detector is, by principle, not competitive with that of specialised high energy resolution semiconductor detectors, it is sufficient for a number of applications. Compared to conventional micro-XRF techniques the developed system allows shortening of the

  8. Total reflection X-ray fluorescence spectrometers for multielement analysis: status of equipment

    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

  9. Portable X-ray fluorescence spectrometer using XR-100CR detector

    Si-PIN photodiode has been being used as radiation detection probe since not long ago. But with obvious advantages as high energy resolution, needless liquid nitrogen and stable operation, this type of probe has been using more and more. The XR100-CR detector including a thermoelectricity cooled Si-PIN photodiode as an X-ray detector, a charge sensitive preamplifier and a novel -30oC temperature regulation electronic circuit is enclosed in a single miniature package. It has small enclosure size (9.5 x 4.4 x 2.9 cm), light weight (125 g), high energy resolution (the 5.9 keV peak of 55Fe is 186 eV FWHM with 20 μs shaping time) and low power consumption (< 1 Watt). With these facilities, this detector is able to use for in-site and outdoor X-ray Fluorescence analysis applications. Nowadays, compact X-ray spectrometers using XR100-CR are installed in factories produce cement, steel, paper, glass and ceramic, etc. to monitor interested chemical elements. Portable X-ray spectrometers are also promoted for outdoor non-destructive analysis of various objects, that we want to know some chemical elements in their composition, such as steel pipes, minerals, antiques and containers, etc. Moreover, electronic devices are more better and specialization with every passing day. The preeminence of XR100-CR detector and modern electronics have been bringing XRF analysis techniques to existence human activities. The portable XRF equipment described in this report is a multifunctional instrument for in-situ, non-destructive and real-time analysis of alloys, minerals, chemicals, papers, and glasses, etc. It was designed by Nuclear Electronics Department (NED) and the XRF group of Radiation Safety and Environment Department, Center for Nuclear Techniques, HCMC. (author)

  10. Analysis of agricultural soils by using energy dispersive X-ray fluorescence

    In this work, we describe an Energy Dispersive x-ray Fluorescence System with a x-ray tube excitation for trace analysis of environmental samples (soil). The system was used to analyze the contamination of metals in treated soils with doses of 10, 20 and 30 ton/ha of compound organic of urban garbage of the type Fertilurb and 10 ton/ha of aviary bed (manure of birds). Samples of roots and foliages of plant radishes cultivated in these soils were also analyzed. The soil samples were collected in five different depths of 0,5, 5-10, 10-20, 20-40 and 40-60 cm. The experimental set-up is composed by an OXFORD X-ray (30 kV, 50 μA and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray spectrum tube is quasi-monochromatic by using of Ti filter. Samples were prepared in pellet form with superficial density in the range of 100 mg/cm2. The fundamental parameter method was used in order to verify the elemental concentration. It was possible to determine the concentrations of thirteen elements: K, Ca, Ti, Mn, Fe, Cu, Zn, Br, Rb, Sr, Y, Zr and Pb in the treated soils with compounds organic. The results indicate that the values found for K, Ca, Rb, Sr, Zr and Pb are significantly above the upper confidence limits for the control soil (α = 0.05). There is a real different between these elements compared to their relationship in the control soils, (α=0,05). There is a real difference between these elements compared to their relationship in the control soils, confirming the influence of the organic compounds in the soil. (author)

  11. Wavelength Dispersive X-ray Fluorescence Spectrometry for the Analysis of Organic Polymer Film

    Recently, many studies have been focused on the thin films because there are numerous industrial processes relevant to thin films such as fuel cells, sensors, lubricants, coatings, and so on. Physical and chemical properties of solid surface have been modified by ultra-thin coatings such as Langmuir-Blodgett (LB) method with a variety of types of organic functional materials for the specific purposes in many applications. In addition, the layer-by-layer technique using polyelectrolyte films are now of interest as biosensors, electrochromic and electroluminescent devices, etc. In general, several methods such as X-ray or neutron reflectivity, and quartz crystal microbalance (QCM) have been utilized for the thin film analysis. These optical techniques can measure the film thicknesses up to hundreds of nanometers while X-ray photoelectron spectroscopy is widely used to study a few nanometers thick films. Other methods such as X-ray Photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atom force microscopy (AFM) have also been used in the film analysis in spite of some disadvantages for each method. X-ray fluorescence (XRF) has long been used as a rapid and simple analytical tool for the analysis of elemental composition of materials. XRF technique is suitable for on-line or in-line real-time monitoring because it is a non-destructive and rapid analysis with good precision and good accuracy at low cost. The aim of this work is to develop a new analytical technique for the quantitative analysis of polymer film on metal substrate. In the present study, Compton peak profile was investigated under different experimental conditions by using wavelength-dispersive XRF (WD-XRF). Compared to energy-dispersive XRF (ED-XRF), WD-XRF is more adequate in an accurate quantitative analysis of thin organic film

  12. Non-destructive in situ study of "Mad Meg" by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    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.

  13. Combined phase and X-Ray fluorescence imaging at the sub-cellular level

    This work presents some recent developments in the field of hard X-ray imaging applied to biomedical research. As the discipline is evolving quickly, new questions appear and the list of needs becomes bigger. Some of them are dealt with in this manuscript. It has been shown that the ID22NI beamline of the ESRF can serve as a proper experimental setup to investigate diverse aspects of cellular research. Together with its high spatial resolution, high flux and high energy range the experimental setup provides bigger field of view, is less sensitive to radiation damages (while taking phase contrast images) and suits well chemical analysis with emphasis on endogenous metals (Zn, Fe, Mn) but also with a possibility for exogenous one's like these found in nanoparticles (Au, Pt, Ag) study. Two synchrotron-based imaging techniques, fluorescence and phase contrast imaging were used in this research project. They were correlated with each other on a number of biological cases, from bacteria E.coli to various cells (HEK 293, PC12, MRC5VA, red blood cells). The explorations made in the chapter 5 allowed preparation of more established and detailed analysis, described in the next chapter where both techniques, X-ray fluorescence and phase contrast imaging, were exploited in order to access absolute metal projected mass fraction in a whole cell. The final image presents for the first time true quantitative information at the sub-cellular level, not biased by the cell thickness. Thus for the first time a fluorescence map serves as a complete quantitative image of a cell without any risk of misinterpretation. Once both maps are divided by each other pixel by pixel (fluorescence map divided by the phase map) they present a complete and final result of the metal (Zn in this work) projected mass fraction in ppm of dry weight. For the purpose of this calculation the analysis was extended to calibration (non-biological) samples. Polystyrene spheres of a known diameter and known

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

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

  15. Characterization of Japanese color sticks by energy dispersive X-ray fluorescence, X-ray diffraction and Fourier transform infrared analysis

    Manso, M. [Centro de Fisica Atomica, Universidade de Lisboa, Faculdade de Ciencias, Av. Prof. Gama Pinto 2, 1649-003 Lisboa (Portugal); Valadas, S. [Chemistry Department, Evora Chemistry Centre and HERCULES Centre, University of Evora, Rua Romao Ramalho, 59 Evora (Portugal); Pessanha, S.; Guilherme, A. [Centro de Fisica Atomica, Universidade de Lisboa, Faculdade de Ciencias, Av. Prof. Gama Pinto 2, 1649-003 Lisboa (Portugal); Queralt, I. [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' , CSIC, Sole Sabaris s/n. 08028 Barcelona (Spain); Candeias, A.E. [Chemistry Department, Evora Chemistry Centre and HERCULES Centre, University of Evora, Rua Romao Ramalho, 59 Evora (Portugal); Carvalho, M.L., E-mail: luisa@cii.fc.ul.p [Centro de Fisica Atomica, Universidade de Lisboa, Faculdade de Ciencias, Av. Prof. Gama Pinto 2, 1649-003 Lisboa (Portugal)

    2010-04-15

    This work comprises the use of energy dispersive X-ray fluorescence (EDXRF), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) techniques for the study of the composition of twentieth century traditional Japanese color sticks. By using the combination of analytical techniques it was possible to obtain information on inorganic and organic pigments, binders and fillers present in the sticks. The colorant materials identified in the sticks were zinc and titanium white, chrome yellow, yellow and red ochre, vermillion, alizarin, indigo, Prussian and synthetic ultramarine blue. The results also showed that calcite and barite were used as inorganic mineral fillers while Arabic gum was the medium used. EDXRF offered great potential for such investigations since it allowed the identification of the elements present in the sample preserving its integrity. However, this information alone was not enough to clearly identify some of the materials in study and therefore it was necessary to use XRD and FTIR techniques.

  16. Cloning, expression, purification and crystallization as well as X-ray fluorescence and preliminary X-ray diffraction analyses of human ADP-ribosylhydrolase 1

    Human ADP-ribosylhydrolase 1, which cleaves the glycosidic bond between ADP-ribose and specific Arg residues in proteins, has been cloned, expressed, purified and crystallized. Human ADP-ribosylhydrolase 1 (hARH1, ADPRH) cleaves the glycosidic bond of ADP-ribose attached to an Arg residue of a protein. hARH1 has been cloned, expressed heterologously in Escherichia coli, purified and crystallized in complex with K+ and ADP. The orthorhombic crystals contained one monomer per asymmetric unit, exhibited a solvent content of 43% and diffracted X-rays to a resolution of 1.9 Å. A prerequisite for obtaining well diffracting crystals was the performance of X-ray fluorescence analysis on poorly diffracting apo hARH1 crystals, which revealed the presence of trace amounts of K+ in the crystal. Adding K-ADP to the crystallization cocktail then resulted in a crystal of different morphology and with dramatically improved diffraction properties

  17. Characterization of the Carancas-Puno meteorite by energy dispersive X-ray fluorescence, X-ray diffractometry and transmission Moessbauer spectroscopy

    Ceron Loayza, Maria L., E-mail: malucelo@hotmail.com; Bravo Cabrejos, Jorge A. [Universidad Nacional Mayor de San Marcos, Laboratorio de Analisis de Suelos, Facultad de Ciencias Fisicas (Peru)

    2011-11-15

    We report the results of the study of a meteorite that impacted an inhabited zone on 15 September 2007 in the neighborhood of the town of Carancas, Puno Region, about 1,300 km south of Lima. The analysis carried out by energy dispersive X-ray fluorescence, X-ray diffractometry and transmission Moessbauer spectroscopy (at room temperature and at 4.2 K), reveal the presence in the meteorite sample of magnetic sites assigned to taenite (Fe,Ni) and troilite (Fe,S) phases, and of two paramagnetic doublets assigned to Fe{sup 2 + }, one associated with olivine and the other to pyroxene. In accord with these results, this meteorite is classified as a type IV chondrite meteorite.

  18. Mineralogical analysis of clays in hardsetting soil horizons, by X-ray fluorescence and X-ray diffraction using Rietveld method

    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. - Highlights: ► Elemental composition of soil samples through X-Ray fluorescence. ► Mineralogical quantification through X-ray diffraction and Rietveld method. ► Oxisol and Ultisol, Brazil ‘Barreiras’ formation. ► High amounts of Si and Al oxides and low amounts of Fe and Ti oxides. ► Predominance of kaolinite in the clay fraction

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

    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 SystemsR 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 iPAQR 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 emit

  20. Heavy metals analysis in fishes by the X-ray fluorescence method

    Among the sources of contamination in human beings we find ingestion of heavy metals. As it is common practice to pour industrial wastes in waters where fishes feed, some toxic elements present in water may pass to human beings through ingestion. It is therefore important to determine the concentrations of heavy metals present in fishes, mainly in those living in waters close to industrial zones or villages. Concentrations of heavy metals in tissue of fishes amount to ppm, hence making necessary the use of very sensitive analytical techniques which do not require a too complex preparation of the sample in order to avoid the loss or contamination of interesting elements of analysis while handling them, thus falsifying the results. The X-Ray Fluorescence method covers these requirements and is not destructive nor multi-elemental. The development of the technique of element analysis in fishes by X-Ray Fluorescence comprised several aspects. from sampling and storage to quantification, specially stressing the preparation of samples. The work was carried out with a Si-Li detector/monitor for solid state and associated electronic equipment. Cd-109 and Pu-238 sources were used to produce excitation, detection limits near 1 ppm were obtained in the majority of elements the technique attained for the analysis of this kind of samples fulfills the celerity, precision, accuracy, and sensitivity requirements. (author)

  1. Analysis of mineral water from Brazil using total reflection X-ray fluorescence by synchrotron radiation

    The total reflection X-ray fluorescence using synchrotron radiation (SRTXRF) has become a competitive technique for the determination of trace elements in samples that the concentrations are lower than 100 ng ml-1. In this work, thirty-seven mineral waters commonly available in supermarkets of Rio de Janeiro, Brazil, were analyzed by SRTXRF. The measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, Sao Paulo, using a polychromatic beam with maximum energy of 20 keV for the excitation. Standard solutions with gallium as internal standard were prepared for calibration of the system. Mineral water samples of 10 μl were added to Perspex sample carrier, dried under infrared lamp and analyzed for 200 s measuring time. It was possible to determine the concentrations of the following elements: Si, S, K, Ca, Ti, Cr, Mn, Ni, Cu, Zn, Ge, Rb, Sr, Ba and Pb. The elemental concentration values were compared with the limits established by the Brazilian legislation

  2. Bromine and bromide content in soils: Analytical approach from total reflection X-ray fluorescence spectrometry.

    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 (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. PMID:27179429

  3. The clumpy torus around type II AGN as revealed by X-ray fluorescent lines

    Liu, Jiren; Li, Xiaobo; Xu, Weiwei; Gou, Lijun; Cheng, Cheng

    2016-01-01

    The reflection spectrum of the torus around AGN is characterized by X-ray fluorescent lines, which are most prominent for type II AGN. A clumpy torus allows photons reflected from the back-side of the torus to leak through the front free-of-obscuration regions. Therefore, the observed X-ray fluorescent lines are sensitive to the clumpiness of the torus. We analyse a sample of type II AGN observed with Chandra HETGS, and measure the fluxes for the Si Ka and Fe Ka lines. The measured Fe Ka/Si Ka ratios, spanning a range between $5-60$, are far smaller than the ratios predicted from simulations of smooth tori, indicating that the tori of the studied sources have clumpy distributions rather than smooth ones. Compared with simulation results of clumpy tori with a half-opening angle of 60$^{\\circ}$, the Circinus galaxy has a Fe Ka/Si Ka ratio of $\\sim60$, which is close to the simulation results for $N=5$, where $N$ is the average number of clumps along the line of sight. The Fe Ka/Si Ka ratios of the other sources...

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

    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. PMID:22846873

  5. Description of CORSET: a computer program for quantitative x-ray fluorescence analysis

    Quantitative x-ray fluorescence analysis requires a method of correcting for absorption and secondary fluorescence effects due to the sample matrix. The computer program CORSET carries out these corrections without requiring a knowledge of the spectral distribution of the x-ray source, and only requires one standard per element or one standard containing all the elements. Sandia's version of CORSET has been divided into three separate programs to fit Sandia's specific requirements for on-line analysis in a melt facility. The melt facility is used to fabricate new alloys with very variable compositions and requires very rapid analyses during a run. Therefore, the standards must be analyzed several days in advance. Program DAT1 is used to set up a permanent file consisting of all the data related to the standards. Program UNINT is used to set up a permanent file with the intensities, background counts and counting times of the unknowns. Program CORSET uses the files created in UNINT and DAT1 to carry out the analysis. This report contains descriptions, listings, and sample runs for these programs. The accuracy of the analyses carried out with these three programs is about 1 to 2% relative with an elemental concentration of about 10 wt %

  6. Precious metal assay analysis of fresh reforming catalyst by x-ray fluorescence spectrometry

    This paper reports that precious metal analysis of fresh reforming catalysts are typically performed by both the catalyst manufacturer and buyer to arrive at a financial settlement on the quantity of metal in each lot of commercial catalyst. Traditional assay methods involve a variety of fire assay or wet chemical acid digestion schemes coupled with gravimetric, colorimetic, or titrimetric measurement for precious metals. Methods must have sufficient precision and accuracy to afford interlaboratory agreement of within one half of one percent relative between the catalyst supplier and purchaser. To meet this requirement many laboratories rely on classical methods. Unfortunately these proceeders are labor intensive and time consuming. X-ray fluorescence has the inherent instrument precision to achieve typical intralaboratory precision of 0.5% RSD on a wide variety of elements and numerous sample types. We have developed an X-ray fluorescence method for the assay quality analysis of fresh reforming catalyst containing platinum, rhenium, and iridium. This method was applied to numerous samples over the past five years

  7. The determination, by x-ray-fluorescence spectrometry, of gold and uranium on resin

    The problems encountered in the determination of gold and uranium that are present simultaneously in a sample of resin were considered, and new background positions, as well as correction factors for background lift and partial spectral overlap, were determined for use in the X-ray-fluorescence measurement of these elements. The agreement between the results obtained by the use of the X-ray-fluorescence method and those obtained by atomic-absorption spectrophotometry were found to be satisfactory. The relative standard deviation in the former measurements is 0,005 at a concentration of 1000 p.p.m., and the working range of the calibrations is 15 to 1000 p.p.m. These limits can be extended by further dilution of the sample. The limits of determination are 6 p.p.m. in the briquette prepared from a sample of resin and 18 p.p.m. in the sample when the maximum mass of the sample is 3 g. The procedure is intended primarily for use in the rapid determination of gold and uranium when no analyses for other elements are required. The time taken for the analysis is 2 hours for 10 samples when 6 standards are used. A computer programme that was developed for the processing of the data is appended as part of a laboratory method

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

    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.

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

    Highlights: •XAFS spectra of Kr have been successfully recorded in irradiated nuclear fuel. •The XAFS data reveal that the next neighbour atoms are Xe. •The estimated density of fission gases is very high and reaches ∼30 nm−3. -- Abstract: 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

  10. Synchrotron Radiation μ-X Ray Fluorescence on Multicellular Tumor Spheroids

    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

  11. Energy dispersive X-ray fluorescence analysis with Bragg polarized Mo radiation

    The aim of introducing energy dispersive analysis into X-ray fluorescence analysis is to suppress background from the Bremsstrahlung spectrum and the characteristic radiation without an undue reduction of the signal. The variant under consideration uses linearly polarization radiation obtained after a Bragg reflection,under delta = 900. In an introductory part, Bragg reflection, fluorescence and strong radiation are considered quantitatively with respect to counting statistics and detection limits. In the experimental part two combinations are describe, of a Ta crystal with a Cr tube and of a Mo crystal with a Mo tube. Details of adjustment, sample preparation and calibration and detection limits are given. The pros and cons of the Ta/Cr and the Mo/Mo are contrasted and proposals for further improvements are given. (G.Q.)

  12. Analysis of stainless steel samples by energy dispersive X-ray fluorescence (EDXRF) spectrometry

    M K Tiwari; A K Singh; K J S Sawhney

    2001-12-01

    A simple method for the analysis of stainless steel samples is presented which is based on radioisotope excited energy dispersive X-ray fluorescence (EDXRF) spectrometry and does not require any type-standards. Both absorption and enhancement effects have been taken into account in the fundamental parameter method for quantitative analysis and an iterative approach is followed for calculation of concentrations in steel samples. Non-linear least square fitting (NL-LSF) procedures have been used to determine accurately the fluorescent peak intensities. The method has been tested by analysing several CRM standard reference samples and 304 and 316 steel samples assuming as unknown. The EDXRF results have also been compared with the results of analysis of same samples by vacuum emission spark spectrometry (VES). Obtained values for concentration in steel samples match quite well with their certified values.

  13. The determination of lanthanum and lanthanide elements by means of X-ray fluorescence analysis

    The quantitative analysis of all lanthanide elements (except Pm) was carried out concurrently using X-ray fluorescence analysis. By choice of suitable preparative methods (thin layer samples prepared by pipetting solutions onto filter paper) and use of an internal standard (Sr) it was possible to obtain linear calibration curves up to high concentrations in the solution (85 g/l) and to suppress disturbances caused by absorption and secondary fluorescence. A correction procedure was developed for reflection superimpositions in the L-spectra of the lanthanide elements which, through selection of the most favourable reflections for analysis, permitted concurrent determination of all 14 elements. Main and secondary constitutents can be analysed whereas enrichment is required for trace analysis. Under routine usage the actual limits of detection range from 3 to 17 μg/cm2 or alternatively 0.3 to 1.7 mg/ml. (orig.)

  14. Optimization of a fluorescence X-ray source and background studies for a prospective CNNS experiment

    Coherent Neutrino Nucleus Scattering (CNNS) is predicted by the Standard Model but hasn't been measured yet. A good background discrimination and shielding is essential for the achievement of a prospective experiment. We show the results of simulations for background discrimination and suppression using a myon veto system in combination with a shielding around a cryostat. With CNNS, the expected nuclear recoil energy for reactor anti-neutrinos is in the range of < or similar 4 keV. Thus a calibration source within this energy region is necessary. Two different methods to create fluorescence are discussed and measured energy spectra will be shown. Finally results of an improved fluorescence x-ray source with nine clearly separated energy lines between ∝1 keV and 6.5 keV are shown.

  15. Data analysis of x-ray fluorescence holography by subtracting normal component from inverse hologram

    X-ray fluorescence holography (XFH) is a powerful technique for determining three-dimensional local atomic arrangements around a specific fluorescing element. However, the raw experimental hologram is predominantly a mixed hologram, i.e., a mixture of hologram generated in both normal and inverse modes, which produces unreliable atomic images. In this paper, we propose a practical subtraction method of the normal component from the inverse XFH data by a Fourier transform for the calculated hologram of a model ZnTe cluster. Many spots originating from the normal components could be properly removed using a mask function, and clear atomic images were reconstructed at adequate positions of the model cluster. This method was successfully applied to the analysis of experimental ZnTe single crystal XFH data. (author)

  16. Micro-electrical discharge machining of 3D micro-molds from Pd40Cu30P20Ni10 metallic glass by using laminated 3D micro-electrodes

    Xu, Bin; Wu, Xiao-yu; Ma, Jiang; Liang, Xiong; Lei, Jian-guo; Wu, Bo; Ruan, Shuang-chen; Wang, Zhen-long

    2016-03-01

    For obtaining 3D micro-molds with better surface quality (slight ridges) and mechanical properties, in this paper 3D micro-electrodes were fabricated and applied to micro-electrical discharge machining (micro-EDM) to process Pd40Cu30P20Ni10 metallic glass. First, 100 μm-thick Cu foil was cut to obtain multilayer 2D micro-structures and these were connected to fit 3D micro-electrodes (with feature sizes of less than 1 mm). Second, under the voltage of 80 V, pulse frequency of 0.2MHZ, pulse width of 800 ns and pulse interval of 4200 ns, the 3D micro-electrodes were applied to micro-EDM for processing Pd40Cu30P20Ni10 metallic glass. The 3D micro-molds with feature within 1 mm were obtained. Third, scanning electron microscope, energy dispersive spectroscopy and x-ray diffraction analysis were carried out on the processed results. The analysis results indicate that with an increase in the depth of micro-EDM, carbon on the processed surface gradually increased from 0.5% to 5.8%, and the processed surface contained new phases (Ni12P5 and Cu3P).

  17. Automation of 3D micro object handling process

    Gegeckaite, Asta; Hansen, Hans Nørgaard

    2007-01-01

    Most of the micro objects in industrial production are handled with manual labour or in semiautomatic stations. Manual labour usually makes handling and assembly operations highly flexible, but slow, relatively imprecise and expensive. Handling of 3D micro objects poses special challenges due to the small absolute scale. In this article, the results of the pick-and-place operations of three different 3D micro objects were investigated. This study shows that depending on the correct gripping t...

  18. Use of x-ray scattering in absorption corrections for x-ray fluorescence analysis of aerosol loaded filters

    Two methods are described for computing multielement x-ray absorption corrections for aerosol samples collected in IPC-1478 and Whatman 41 filters. The first relies on scatter peak intensities and scattering cross sections to estimate the mass of light elements (Z less than 14) in the sample. This mass is used with the measured heavy element (Z greater than or equal to 14) masses to iteratively compute sample absorption corrections. The second method utilizes a linear function of ln(μ) vs ln(E) determined from the scatter peak ratios and estimates sample mass from the scatter peak intensities. Both methods assume a homogeneous depth distribution of aerosol in a fraction of the front of the filters, and the assumption is evaluated with respect to an exponential aerosol depth distribution. Penetration depths for various real, synthethic and liquid aerosols were measured. Aerosol penetration appeared constant over a 1.1 mg/cm2 range of sample loading for IPC filters, while absorption corrections for Si and S varied by a factor of two over the same loading range. Corrections computed by the two methods were compared with measured absorption corrections and with atomic absorption analyses of the same samples

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

    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 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−1 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 and with iterative maximum-likelihood expectation maximization without and with attenuation correction. While K-shell XFCT was capable of providing an 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 the 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−1 could be imaged with L-shell XFCT inside a 2 cm and 4 cm diameter object, respectively. (paper)

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

    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

  1. Medieval glass from the Cathedral in Paderborn: a comparative study using X-ray absorption spectroscopy, X-ray fluorescence, and inductively coupled laser ablation mass spectrometry

    We have investigated four stained glass samples recovered from an archaeological excavation at the Cathedral in Paderborn (Germany) between 1978 and 1980. On two of the samples there are parts of paintings. Concentrations of major elements were determined using two independent techniques: LA-ICP-MS (a UV laser ablation microsampler combined with an inductively coupled plasma mass spectrometer) and synchrotron radiation X-ray excited X-ray fluorescence (SR-XRF). The SR-XRF data were quantified by using the program package PyMCA developed by the software group of the ESRF in Grenoble. Significant differences were found between the concentrations determined by the two techniques that can be explained by concentration gradients near the surface of the glasses caused, for example, by corrosion/leaching processes and the different surface sensitivities of the applied techniques. For several of the elements that were detected in the glass and in the colour pigments used for the paintings X-ray absorption near edge structure (XANES) spectra were recorded in order to determine the chemical speciation of the elements of interest. As was expected, most elements in the glass were found as oxides in their most stable form. Two notable exceptions were observed: titanium was not found as rutile - the most stable form of TiO2 - but in the form of anatase, and lead was not found in one defined chemical state but as a complex mixture of oxide, sulphate, and other compounds. (orig.)

  2. Medieval glass from the Cathedral in Paderborn: a comparative study using X-ray absorption spectroscopy, X-ray fluorescence, and inductively coupled laser ablation mass spectrometry

    Hormes, J. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Louisiana State University, CAMD, Baton Rouge, LA (United States); Roy, A.; Bovenkamp, G.L. [Louisiana State University, CAMD, Baton Rouge, LA (United States); Simon, K. [University of Goettingen, Geochemistry, Centre for Geosciences, Goettingen (Germany); Kim, C.Y. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Boerste, N. [Faculty for Theology Paderborn, Paderborn (Germany); Gai, S. [LWL - Archaeologie fuer Westfalen, Muenster (Germany)

    2013-04-15

    We have investigated four stained glass samples recovered from an archaeological excavation at the Cathedral in Paderborn (Germany) between 1978 and 1980. On two of the samples there are parts of paintings. Concentrations of major elements were determined using two independent techniques: LA-ICP-MS (a UV laser ablation microsampler combined with an inductively coupled plasma mass spectrometer) and synchrotron radiation X-ray excited X-ray fluorescence (SR-XRF). The SR-XRF data were quantified by using the program package PyMCA developed by the software group of the ESRF in Grenoble. Significant differences were found between the concentrations determined by the two techniques that can be explained by concentration gradients near the surface of the glasses caused, for example, by corrosion/leaching processes and the different surface sensitivities of the applied techniques. For several of the elements that were detected in the glass and in the colour pigments used for the paintings X-ray absorption near edge structure (XANES) spectra were recorded in order to determine the chemical speciation of the elements of interest. As was expected, most elements in the glass were found as oxides in their most stable form. Two notable exceptions were observed: titanium was not found as rutile - the most stable form of TiO{sub 2} - but in the form of anatase, and lead was not found in one defined chemical state but as a complex mixture of oxide, sulphate, and other compounds. (orig.)

  3. Minority additive distributions in a ceramic metal-halide arc lamp using high-energy x-ray induced fluorescence

    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

  4. Minority additive distributions in a ceramic metal-halide arc lamp using high-energy x-ray induced fluorescence

    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.

  5. L2,3 subshell X-ray fluorescence yields and Coster-Kronig transition probabilities of Nd and Yb

    X-ray spectra emitted in the radioactive decay of 17.7y 145Pm and 1.9y 171Tm were studied using a three-parameter technique for XX.t coincidence measurements. The following L2 and L3 subshell X-ray fluorescence yields, ω2, ω3, Coster-Kronig transition probabilities, f23, and radiative decay branching ratios, s2, s3, were determined for Nd (Z=60) and Yb (Z=70). (orig./WL)

  6. X-ray fluorescence study of organic-inorganic polymer conversion into ceramics induced by ion irradiation

    Kurmaev, E. Z.; Moewes, A.; Krietemeyer, M.; Endo, K; Ida, Tomonori; Shimada, S.

    1999-01-01

    Changes to the local and electronic structures of phenyltriethoxysilane ~PTES! films when irradiated at room temperature with gold ion concentrations of 531014 to 2.531015 cm22 and with carbon ion concentrations of 531015 cm22 were studied using x-ray emission and photoelectron spectroscopies. The fluorescent ultrasoft silicon LII,III and carbon Ka x-ray emission spectra of unirradiated and irradiated PTES films were measured at the Advanced Light Source, and the Center for Advanc...

  7. Considerations on the ideal sample shape for Total Reflection X-ray Fluorescence Analysis

    Total Reflection X-ray Fluorescence analysis (TXRF) is widely used in semiconductor industry for the analysis of silicon wafer surfaces. Typically an external standard is used for the calibration of the spectrometer. This is sensitive to errors in quantification. For small sample amounts the thin film approximation is valid, absorption effects of the exciting and the detected radiation are neglected and the relation between sample amount and fluorescence intensity is linear. For higher total sample amounts deviations from linearity have been observed (saturation effect). These deviations are one of the difficulties for external standard quantification. A theoretical determination of the ideal TXRF sample shape is content of the presented work with the aim to improve the calibration process and therefore the quantification. The fluorescence intensity emitted by different theoretical sample shapes was calculated, whereby several parameters have been varied (excitation energy, density, diameter/height ratio of the sample). It was investigated which sample shape leads to the highest fluorescence intensity and exhibits the lowest saturation effect. The comparison of the different sample shapes showed that the ring shape matches the ideal TXRF sample shape best. - Highlights: ► In this work the ideal TXRF sample shape is theoretically determined. ► Different theoretical sample shapes were investigated. ► The ring shape matches the ideal TXRF sample shape best. ► It leads to the highest fluorescence intensity and the lowest saturation effect.

  8. In vivo elemental analysis in occupational medicine using X-ray fluorescence

    A technique for the in vivo determination of cadmium in the kidney cortex using X-ray fluorescence analysis (XRF) has been developed for clinical use. The method uses the Cd K-alfa X-rays. The radiation from the tube was polarized by scattering at 90 degrees in a plastic disc. Using a Si(Li) detector the minimum detectable concentration (MDC) of cadmium in the renal cortex was about 6 ppm for an effective dose equivalent of 3 micro-Sievert. The precision of the method was estimated to be about 23 percent. The clinical usefulness was confirmed by studying 20 occupationally exposed cadmium workers and three controls. The cadmium workers showed levels of cadmium in the kidney in the range 47-317 ppm, and controls showed levels below 30 ppm. Using XRF in vivo large-scale measurements of lead in the fingerbone of more than 100 lead workers were performed. The technique used included two 57-Co sources for excitation and a higher-purity Ge detector for the analysis of the Pb K-alfa X-rays. The MDC was about 20 ppm for an effective dose equivalent of 0.1 micro-Sievert. The precision of the method was estimated to be about 15 per cent. The in vivo measurements showed levels of fingerbone-Pb up to 148 ppm. The existence of a significant endogenous exposure from lead in the skeleton was confirmed. The fingerbone-Pb was correlated to time-integrated blood-Pb indicating that it could be used as a rough estimated of time-integrated exposure. The results from the measurements were used to develop a three-compartment (cortical bone, trabecular bone, blood/soft tissues) model. Using this model, lead levels in fingerbone, vertebrae and blood could be predicted in good agreement with observations. (author)

  9. Resonant inelastic scattering in dilute magnetic semiconductors by x-ray fluorescence spectroscopy

    Lawniczak-Jablonska, K. [Lawrence Berkeley National Lab., CA (United States)]|[Institute of Physics, Warsaw (Poland); Jia, J.J.; Underwood, J.H. [Lawrence Berkeley National Lab., CA (United States)] [and others

    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.

  10. Simulated 'On-Line' Wear Metal Analysis of Lubricating Oils by X-Ray Fluorescence Spectroscopy

    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.

  11. X-ray fluorescence analysis in environmental radiological surveillance using HPGe detectors

    X-ray fluorescence (XRF) has been proven to be a valuable tool for determining trace quantities of heavy metals, such as uranium and lead, in different types of samples. The present paper demonstrates the applicability of XRF spectrometry to measure the concentrations of these heavy metals in samples from natural ore and soil. The values of uranium concentrations in rock from the Pena Blanca uranium ore, in Chihuahua, Mexico, were calculated for the purpose of precertifying the rock powders samples. The comparison with other techniques, such as inductively coupled plasma atomic emission spectrometry, atomic absorption spectrometry, alpha spectrometry and electron microscopy, was used to complete the precertification process, so that the sample powders may be used as secondary standards. The source-sample-detector geometry and the incident angle are the most important factors for obtaining low detection limits. The selected system uses a 57Co source of about 0.1 mCi to excite the K X-rays from uranium and lead. X-rays were recorded on a CANBERRA HPGe coaxial detector. The comparative results for two incident angles (90 deg and 180 deg ) performed previously by other authors show that the best geometry is the backscattering geometry. In the present paper, using EGS4 code system with Monte Carlo simulation, it was possible to determine the location and distribution of background produced by the Compton edge in the optimized geometry. This procedure allowed to find the minimum detectable concentration of uranium and lead, which was experimentally calculated using standards. The possibility of performing in vivo measurements rapidly and easily, as well as the factors affecting accuracy and the minimum detectable concentration in several samples are also discussed

  12. Quantification of metals in lipstick by energy dispersive X-ray fluorescence

    Full text: The objective of this work is to analyze lipstick and lip balm by Energy Dispersive X-Ray Fluorescence and verify if the concentration of the found elements are in accordance with federal rules. Two lip balm and 30 lipstick commercially available were analyzed without preparation. The samples were rubbed on a mylar film until they form a relatively homogeneous layer over entire surface of the film. The superficial density of the samples ranged from 0,0004 to 0,015 g cm-2 , which characterize thin film geometry. Sensitivity values were determined using MicroMatter standards. The measurement system, from Applied Nuclear Physics Laboratory of UEL, consists in a Si-PIN X-ray detector (221 eV resolution for 5,9 keV line, 25 μm Be window) and a mini X-ray tube (4W, Ag target, 50 μm Ag filter). One of the lip balm presented 2620 ± 477 μg g-1 of Ti and in the other sample none inorganic elements, which characterize a formulation based on organic compounds. In the lipstick were found the following elements and the number of samples in which it appears, with its respective range of concentration in μg g-1: Ti (17) 691 to 12721, Fe (22) 237 to 16377, Zn (3) 105 to 2850, Br (2) 510 to 3097, Sr(4) 254 to 1170, Ba (2) 58170 to 90506 and Bi (1) 16275 ± 798. According to Brazilian federal rules (ANVISA 79.094) it is not permitted the presence of As and Pb in the formulations. The methodology demonstrated to be suitable for quantification of metals at in natura samples of lipsticks, discarding sample preparation. In sequence a detailed study of the influence of these elements on human health will be performed. (author)

  13. Quantification of metals in lipstick by energy dispersive X-ray fluorescence

    Wouk, Luana Cristina; Melquiades, Fabio Luiz [Universidade Estadual do Centro Oeste (UNICENTRO), PR (Brazil). Dept. de Fisica

    2011-07-01

    Full text: The objective of this work is to analyze lipstick and lip balm by Energy Dispersive X-Ray Fluorescence and verify if the concentration of the found elements are in accordance with federal rules. Two lip balm and 30 lipstick commercially available were analyzed without preparation. The samples were rubbed on a mylar film until they form a relatively homogeneous layer over entire surface of the film. The superficial density of the samples ranged from 0,0004 to 0,015 g cm{sup -2} , which characterize thin film geometry. Sensitivity values were determined using MicroMatter standards. The measurement system, from Applied Nuclear Physics Laboratory of UEL, consists in a Si-PIN X-ray detector (221 eV resolution for 5,9 keV line, 25 {mu}m Be window) and a mini X-ray tube (4W, Ag target, 50 {mu}m Ag filter). One of the lip balm presented 2620 {+-} 477 {mu}g g{sup -1} of Ti and in the other sample none inorganic elements, which characterize a formulation based on organic compounds. In the lipstick were found the following elements and the number of samples in which it appears, with its respective range of concentration in {mu}g g{sup -1}: Ti (17) 691 to 12721, Fe (22) 237 to 16377, Zn (3) 105 to 2850, Br (2) 510 to 3097, Sr(4) 254 to 1170, Ba (2) 58170 to 90506 and Bi (1) 16275 {+-} 798. According to Brazilian federal rules (ANVISA 79.094) it is not permitted the presence of As and Pb in the formulations. The methodology demonstrated to be suitable for quantification of metals at in natura samples of lipsticks, discarding sample preparation. In sequence a detailed study of the influence of these elements on human health will be performed. (author)

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

    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 (III 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

  15. X-ray fluorescence in Member States: Argentina. Characterization of black vulcanites coming from Rincon Chico 2 site, Neuquen, Argentina, by using X-ray fluorescence spectrometry

    Full text: The investigation of prehistoric hunter-gatherers archaeological sites in the Limay river basin (provinces of Neuquen and Rio Negro) raised different questions concerning the lithic technology. In Rincon Chico 2, a site located on the margin of the Limay river in the Neuquen province and nowadays submerged by the Piedra del Aguila reservoir, many tools and debitage made in black volcanic rock has been found. The identification of this raw material can give information about possible sources of provenance. The rocks were classified macroscopically either as basalt (with coarse grains) or dacite (with fine grains) However, in several cases, a dual behaviour was observed in the fracture zone: the texture was coarse on the surface and very fine, sometimes almost vitreous, in the interior. Following this observation, it was decided to introduce a new more general category called 'black vulcanites'. Looking for the origin and more precise identification of this raw material, artifactual samples and a set of black vulcanite fragments coming from Paso Limay, a dacite source located 50 km from the archaeological site, were characterized by X-ray fluorescence spectrometry using a Philips Minipal energy dispersive system. Samples were analysed as loose powder. Statistical analysis reveals greater variability between artefact samples than between the samples from the source itself. This discrepancy is more evident if Fe, Ti and Zn are used as markers. These results suggests that the quarry at Paso Limay was not the main source of provenance of the black vulcanites utilized by the hunter-gatherers occupying Rincon Chico. (author)

  16. Detection of Fingerprints Based on Elemental Composition Using Micro-X-Ray Fluorescence.

    Worley, C. G. (Christopher G.); Wiltshire, S. (Sara); Miller, T. C. (Thomasin C.); Havrilla, G. J. (George J.); Majidi, V. (Vahid)

    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

  17. Ambiental applications of Total Reflection X-Ray Fluorescence in Mexico

    Full text: The National Institute of Nuclear Investigations, through the Management of Environmental Sciences has recently acquired a Total Reflection X Ray Fluorescence equipment, Ital Structures I T-2000. This is the first reflection equipment that operates in Mexico, and it allows to increase the analytic capacity in the environmental surface area of the country. This completely automated equipment is used in the environmental samples analysis, which means natural and wastewaters, silts and soils, blood, urine, fish, plankton, vegetables, filters with particulated matter, among other, using as quantification method the one called internal standard. The limits of detection vary from 4 up to 100 μg/L depending of the element and the used x-rays tube. This equipment allows to give support to different projects related with the contamination and the environmental protection in Mexico, just as the study of the distribution heavy metals in water and silt from different bodies of water, the metal accumulation in plankton, aquatic flowers, fish and birds, the study of particulate matter in Mexico City atmosphere, and in the identification of heavy metals in ground waters polluted with leached derived from mining industry

  18. Deformulation of a solid pharmaceutical form using computed tomography and X-ray fluorescence

    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.

  19. The description of compton lines in energy-dispersive x-ray Fluorescence

    Energy-Dispersive X-Ray Fluorescence (ED-XRF) is a non-destructive technique for the element analysis in a concentration range ppm - % making use of X rays up to 100 keV. Generally, two photon matter interactions occur, respectively absorption and scattering. The absorption of incident photons gives raise to characteristic lines. Scattering gives an incoherent and a coherent line. A Gaussian peak model is adequate to describe the characteristic and coherent scattered lines. Incoherent lines appear as non-Gaussian, broadened peaks. The profile of a Compton peak is complex. It depends on the geometry and the composition of the sample. Especially, when analyzing a low Z matrix; dominant scattering and multiple scattering may cause large interferences. The absence of an appropriate fitting model makes the Compton profile seen as a limiting factor in the evaluation of spectra. An accurate description of incoherent lines should improve quantitative analysis. Therefore, a suitable fitting model, making use of the expertise of non-linear least squares procedures and Monte-Carlo calculations was systematically investigated. The proposed model, containing a modified Gaussian, is tested on experimental data recorded with a HPGe detector

  20. Radiography and X-ray fluorescence used to analyze cultural and artistic artifacts

    Since 2003 the analyses of artistic and cultural heritage objects at LAMFI-USP (Laboratorio de Analises de Materiais com Feixes Ionicos), initially restricted to ion beam methods, are growing steadily. Since then, alternative methodologies and procedures have been incorporated to better characterize these objects, which possess distinct physical characteristics and also high cultural and monetary value. The examinations in this kind of objects were expanded to other non-destructive analytical techniques like portable EDXRF (Energy Dispersive X-ray Fluorescence) analysis, X-ray radiography, visible photography, UV (ultraviolet) and IR (infrared) light imaging that are helping to better understand these art objects, particularly paintings. These techniques are helping the analyses of the conservation state of the objects and also revealing characteristics of the painter such as underlying drawings, which help understand the creative process of the artist. These new procedures of analysis are aimed to enable better analytic research in archaeology and artistic and cultural heritage objects and to provide results that subsidize authentic investigations of art objects as well as the origin of archaeological artifacts, while stimulating archeometry and 'arteometry' research in Brazilian Museums. (author)

  1. Elemental analysis of crude and lubricating oils by energy dispersive x-ray fluorescence

    This paper reports that most aspects of petroleum research, exploration, and refining require elemental analysis from trace to minor elemental concentrations. Numerous elements ranging from atomic numbers 15 to 92 can be found in many crudes. Elements such as vanadium, iron, nickel, copper, and arsenic can have deleterious effects on the catalysts utilized in the catalytic cracking process. Other elements purposely introduced as additives into finished lubricating oils must also be measured and controlled. Typically elements such as phosphorus, sulphur, calcium, zinc, and molybdenum are in the range of 0.00 to 5.00 wt%. In addition to crude oils and finished lubricating oils, engine and turbine bearing wear analysis are often performed by X-ray fluorescence. In these cases, typical bearing and piston ring elements such as copper, chromium, zinc, lead, tin, and silver are usually quantified. The techniques for preparing samples of crude oil, finished lubricating oils, and used engine oils are basically identical. The sample is transferred into the polypropylene sample cup with a 6.3 μm polypropylene support film. Errors in volume or sample depth can produce significant intensity deviations for higher energy X-rays. The error for lead, for example, is approximately 1.5% relative per 0.1 mL error at volumes of 3 mL. Minimum detectable limits or several tenths of parts per million for atomic numbers 30 to 92 from a range of 5 to 800 parts per million can be expected

  2. In vivo monitoring of toxic metals: assessment of neutron activation and x-ray fluorescence techniques

    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

  3. Energy dispersive X-ray fluorescence from useless tyres samples with a Si PIN detector

    The concentration of Zn from discard tyre samples is of environmental interest, since on its production are used S for the rubber vulcanization process, and Zn O as reaction catalyze. The useless tyres are been used for asphalt pave, burn in cement industry and thermoelectric power plant and in erosion control of agriculture areas. Analyses of these samples requires frequently chemical digestion that is expensive and take a long time. Trying to eliminate these limitations, the objective of this work was use Energy Dispersive X Ray Fluorescence technique (EDXRF) with a portable system as the technique is multi elementary and needs a minimum sample preparation. Five useless tyres samples were grind in a knife mill and after this in a cryogenic mill, and analyzed in pellets form, using a X ray mini tube (Ag target, Mo lter, 25 kV/20 A) for 200 s and a Si-PIN semiconductor detector coupled to a multichannel analyzer. Were obtained Zn concentrations in the range of 40.6 to 44.2 g g1, representing nearly 0.4. (author)

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

    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.

  5. A multi-channel monolithic Ge detector system for fluorescence x-ray absorption spectroscopy

    Bucher, J.J.; Allen, P.G.; Edelstein, N.M.; Shuh, D.K. [Lawrence Berkeley National Lab., CA (United States). Chemical Sciences Div.; Madden, N.W.; Cork, C.; Luke, P.; Pehl, D.; Malone, D. [Lawrence Berkeley National Lab., CA (United States). Engineering Div.

    1995-03-01

    Construction and performance of a monolithic quad-pixel Ge detector for fluorescence x-ray absorption spectroscopy (XAS) at synchrotron radiation sources are described. The detector semiconductor element has an active surface area of 4.0 cm{sup 2} which is electrically separated into four 1.0 cm{sup 2} pixels, with little interfacial dead volume. Spatial response of the array shows that cross-talk between adjacent pixels is < 10% for 5.9 keV photons that fall within 0.5 mm of the pixel boundaries. The detector electronics system uses pre-amplifiers built at LBNL with commercial Tennelec Model TC 244 amplifiers. Using an {sup 55}Fe test source (MnK{sub {alpha}}, 5.9 keV), energy resolution of better than 200 eV is achieved with a 4 {mu}sec peaking time. At 0.5 {mu}sec peaking time, pulse pileup results in a 75% throughput efficiency for an incoming count rate of 100 kHz. Initial XAS fluoresncece measurements at the beamline 4 wiggler end stations at SSRL show that the detector system has several advantages over commercial x-ray spectrometers for low-concentration counting.

  6. Radiography and X-ray fluorescence used to analyze cultural and artistic artifacts

    Rizzutto, Marcia A.; Kajiya, Elizabeth M.; Campos, Pedro H.O.V. de; Almeida, Paula A.D., E-mail: rizzutto@if.usp.br, E-mail: elizabethkajiya@gmail.com [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil)

    2013-07-01

    Since 2003 the analyses of artistic and cultural heritage objects at LAMFI-USP (Laboratorio de Analises de Materiais com Feixes Ionicos), initially restricted to ion beam methods, are growing steadily. Since then, alternative methodologies and procedures have been incorporated to better characterize these objects, which possess distinct physical characteristics and also high cultural and monetary value. The examinations in this kind of objects were expanded to other non-destructive analytical techniques like portable EDXRF (Energy Dispersive X-ray Fluorescence) analysis, X-ray radiography, visible photography, UV (ultraviolet) and IR (infrared) light imaging that are helping to better understand these art objects, particularly paintings. These techniques are helping the analyses of the conservation state of the objects and also revealing characteristics of the painter such as underlying drawings, which help understand the creative process of the artist. These new procedures of analysis are aimed to enable better analytic research in archaeology and artistic and cultural heritage objects and to provide results that subsidize authentic investigations of art objects as well as the origin of archaeological artifacts, while stimulating archeometry and 'arteometry' research in Brazilian Museums. (author)

  7. Semiconductor Si(Li)-spectrometer with thermoelectric cooling for X-ray fluorescence logging

    A miniature silicon-lithium spectrometer has been developed in Leningrad University. The spectrometer consists of a well device, 36 mm in diameter and 1200 mm heigh, cable and terrestrial equipment set. Power supply to thermoelectric battery (15 mV) from the surface of power supply rectifier connected with the cable through a decoupling device is a specific feature of the spectrometer. Amplifier and pulse-height analyzer consisting of specially developed discriminators and a ratio meter are the main components of the terrestrial equipment set. The circuit of analysis block discriminators of an automatic X-ray radiometric fluorescence analyzer is used as the basis for discriminators. To facilitate measurements of spectra and determination of amplifier formation constants a multichannel pulse analyzer, digit printing block and oscillograph have been introduced in the composition of the terrestrial equipment. The spectrometer has been tested in rising and horizontal holes of underground drilling at gold-silver deposit. Test results confirm the prospects of the application of X-ray logging spectrometers with Si(Li) semiconductor detectors in geology and mining. The spectrometer block diagram as well as roentgenooptic sensor diagram with Si(Li) semiconductor detector and well logs are presented

  8. Optimizing the operation of a high resolution vertical Johann spectrometer using a high energy fluorescer x-ray source

    This paper describes the operation and testing for a vertical Johann spectrometer (VJS) operating in the 13 keV range. The spectrometer is designed to use thin curved mica crystals or thick germanium crystals. The VJS must have a resolution of E/ΔE=3000 or better to measure the Doppler broadening of highly ionized krypton and operate at a small x-ray angle in order to be used as a diagnostic in a laser plasma target chamber. The VJS was aligned, tested, and optimized using a fluorescer type high energy x-ray (HEX) source located at National Security Technologies (NSTec), LLC, in Livermore, CA. The HEX uses a 160 kV x-ray tube to excite fluorescence from various targets. Both rubidium and bismuth fluorescers were used for this effort. This presentation describes the NSTec HEX system and the methods used to optimize and characterize the VJS performance.

  9. The use of multilayer monochromators and rotating-anode X-ray tubes in total-reflection X-ray fluorescence analysis

    Total-reflection x-ray fluorescence analysis (TXRF) has become a powerful analytical tool for ultra trace element analysis down to the ppt - level (parts per trillion). A further improvement of the method is achieved by monoenergetic excitation of the sample using synthetic multilayer structures as monochromators. These multilayers are better suited than crystal monochromators in TXRF due to their broader relative energy bandwidth. Advantages and disadvantages of using a W/C multilayer structure in TXRF are discussed. A new multifunctional vacuum chamber was constructed to compare monoenergetic and full spectrum excitation under optimized measuring geometries using rotating and standing anode x-ray tubes as primary radiation sources. Detection limits (extrapolated for a measuring time of 1000 s) of 170 femtogram (170 x 10-15 g) were obtained for the element Mn with full spectrum excitation (rotating Cu-anode). The quantitative analysis is substantially simplified applying monoenergetic excitation since fundamental parameters from tables can be used for elemental sensitivities. No more multielement standards are necessary for establishing calibration curves. Corrections for absorption of the fluorescence radiation in the sample can be neglected due to minute sample masses in TXRF (thin film approximation). The excitation energy is tuned by the multilayer using the bremsstrahlung and characteristic lines of different anode materials (W, Mo) to obtain selective excitation of certain elements in the sample. The multilayer monochromator is compared to total-reflection high energy cut-off filters as a device for modifying the primary spectrum

  10. Standard test methods for chemical analysis of ceramic whiteware materials using wavelength dispersive X-Ray fluorescence spectrometry

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO, and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. (1) In addition to 10 major elements, the method provides a gravimetric loss-on-ignition. Note 1—Much of the text of this test method is derived directly from Major element analysis by wavelength dispersive X-ray fluorescence spectrometry, included in Ref (1). 1.2 Interferences, with analysis by WDXRF, may result from mineralogical or other structural effects, line overlaps, and matrix effects. The structure of the...

  11. Energy-dispersive x-ray-fluorescence analysis for on-line uranium-concentration measurement

    An on-line monitor capable of near-real-time measurement of uranium concentrations in process streams has been developed and demonstrated. The monitor, which uses energy dispersive x-ray fluorescence analysis techniques, has been evaluated in the laboratory and in a solvent extraction column study using natural uranium. Concentrations in the range 0.5 to 150 g/l have been measured in both flowing aqueous and organic streams. For streams with uranium concentrations in the range 20 to 150 g/l, data collection times of 300 seconds are sufficient to measure the concentration with less than 2% error. Streams which have lower concentrations require longer data collection times to provide the same measurement error. The results are used for nuclear material inventory and process control

  12. X-Ray fluorescence of microquantities of hafnium in zirconium by precipitation as thin film

    The importance of Zr and Hf in the nuclear industry represents and increasing need for the development of reliable chemical methods to determine Hf traces in Zr matrix. A precipitation method in amoniacal medium was developed. A thin film is obtained where matrix effects are absent or minimized. Hf in the range of 5-70.10-9Kg in a 5.10-6Kg Zr matrix was studied. Fluorescence Hf Lα and Hf Lβ X-rays are excited by a W-anode tube 17 kV-25mA and 50kV-25mA. Radiation scattered by the tube was used as internal standard. Bartlett criterion was used for the regression analysis. Determination limit was fixed in 5±4. 10-9Kg Hf at a 95 % probability. (Author)

  13. Use of X-ray fluorescence analysis for the determination of hafnium in zircalloys

    The determination of hafnium at trace levels (ppm) in the presence of zirconium by X-ray fluorescence technique is presented. The samples were prepared in the form of double-layer pellets, with boric acid as the binding material. The most sensitive first order line of hafnium HfLα (0.157 nm), which is used analyticaly, has approximately 67% overlapping with second order line of zirconium ZrKα1, (0.079 nm). As the excitation potencial of zirconium is larger than hafnium, the best condition was selected, so that the interference of zirconium intensity would not be significant in hafnium analytical line. The method allowed the determination of hafnium above 5.0 ppm (LLd = 1.5 ppm) with an accuracy of less than 10%. (Author)

  14. Instrumental aspects of tube-excited energy-dispersive X-ray fluorescence analysis

    Energy-dispersive X-ray fluorescence spectrometry is an attractive and widely used method for sensitive multi-element analysis. The method suffers from the extreme density of spectral components in a rather limited energy range which implies the need for computer based spectrum analysis. The method of iterative least squares analysis is the most powerful tool for this. It requires a systematic and accurate description of the spectral features. Other important necessities for accurate analysis are the calibration of the spectrometer and the correction for matrix absorption effects in the sample; they can be calculated from available physical constants. Ours and similar procedures prove that semi-automatic analyses are possible with an accuracy of the order of 5%. (author)

  15. Accuracy of X-ray fluorescence spectrometric determination of Rb and Sr concentrations in rock samples

    It is shown that application of the Compton scattering for matrix correction in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide concentrations at a relative accuracy level of 1%. The empirical method applies to rock samples showing differences in mass absorption up to a factor of two. The accuracy of the method has been tested by analysis of 57 samples analysed for Rb and Sr by mass spectrometric isotope dilution. In addition a few of the U.S. Geological Survey reference rock powders, showing significantly different mass absorption, were analysed for Rb and Sr. It is demonstrated that the mica effect, if significant, is smaller than 1% relative. There is no advantage in the use of the LiF(220) analysing crystal as a substitute for the LiF(200). The method appears to be insensitive to the pellet thickness. (author)

  16. Determination of thorium in concentrates from monazite sand by X-ray fluorescence technique

    A method for the determination of thorium by X-ray fluorescence technique in concentrates obtained from monazite sand is outlined. The fusion-dilution method is used for the sample preparation. The sample in the original form is mixed with a fusion flux. After fusion of the mixture a pellet with smooth surface is obtained. No chemical separation procedure is necessary. The intensity of the Thlα line is used for the calculation of the thorium content in the sample with the aid of the double dilution method. A good reproducibility is observed for the thorium determination in the concentrate; the precision observed is of the order of + - 1.85%. (Author)

  17. Trace element distribution in human teeth by x-ray fluorescence spectrometry and multivariate statistical analysis

    Oprea, Cristiana; Gustova, Marina V; Oprea, Ioan A; Buzguta, Violeta L

    2014-01-01

    X-ray fluorescence spectrometry (XRFS) was used as a multielement method of evaluation of individual whole human tooth or tooth tissues for their amounts of trace elements. Measurements were carried out on human enamel, dentine, and dental cementum, and some differences in tooth matrix composition were noted. In addition, the elemental concentrations determined in teeth from subjects of different ages, nutritional states, professions and gender, living under various environmental conditions and dietary habits, were included in a comparison by multivariate statistical analysis (MVSA) methods. By factor analysis it was established that inorganic components of human teeth varied consistently with their source in the tissue, with more in such tissue from females than in that from males, and more in tooth incisor than in tooth molar.

  18. Total reflection X-ray fluorescence analysis of airborne particulate matter

    Klockenkaemper, R.; Bayer, H.; Bohlen, A. von [Institut fuer Spektrochemie und Angewandte Spektroskopie, Dortmund (Germany)

    1995-03-01

    The collection of air dust by a `Berner`- and a `Battelle`-impactor was adapted to the subsequent analysis by Total reflection X-Ray Fluorescence (TXRF). A suitable impactor material has to be chosen in order to avoid high blank values, collection losses and memory effects. Stainless steel even coated by TiN is not at all suitable. Titanium and aluminium are less favourable than makrolon or another high polymer which may even be antistatic. Small sampling volumes of only 1 m{sup 3} and short sampling times of about 1 h are sufficient for a multielement analysis by TXRF. Low detection limits of ng/m{sup 3} and a repeatability of some % can be realized. (author).

  19. X-ray fluorescence analysis of trace elements in blood serum from diabetic patients

    Full text: The wave dispersive X-ray fluorescence (WDXRF) technique was used for analysis of trace elements in blood serum from 23 nondiabetic healthy individuals (control group) and 58 type II diabetic patients who attended the diabetic clinics. The elements Na, Mg, Al, P, S, Cl, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Se, Mo, Cd, Hg and Pb were identified and their concentrations were estimated. Physical basis of used analytical methods, experimental set-up and the procedure of sample preparation are described. The maximum increase in trace elements in the blood samples of the workers compared with the control group was observed for Pb but also for Rb, As and Br

  20. Determination of rubidium and strontium in geological materials by X-Ray fluorescence spectrometry

    In order to determine whole-rock ages by the Rb/Sr procedure, an X-ray fluorescence spectrometry method for the determination of both elements has been developed. The samples are pressed into boric acid backed and ringed pellets with this material as a binding agent. Matrix corrections are made following the determination od the mass absorption coefficients, based on the intensity of the Compton-scattered peak of MoKα. or MoKβ1.3. The U. S. Geological Survey granodiorite GSP-1 is used as a reference standard. Spectral-line interferences have been carefully studied and the empirical correction factors determined. A BASIC language program for calculating the Rb and Sr concentrations and the Rb/Sr ratios has been written. (Author) 7 refs

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

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

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

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

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

    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. X-Ray Fluorescence to Determine Zn in Bolivian Children using Hair Samples

    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

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

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

    2014-11-01

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

  6. Procedure of trace element analysis in oyster tissues by using X-ray fluorescence

    The procedure of trace element analysis such as Ca, Mn, Fe, Zn, Cu, Pb in molluscs (oyster tissues) was established by using X-ray fluorescence techniques. The procedure was investigated from the sample collection, drying, ashing ratio to the analytical techniques by using Cd-109, detector Si (Li) and the peak processing MCAPLUS program was applied for this study. The procedure is based on direct comparison with certified concentrations of international standard reference SRM 1566b Oyster Tissue of National Institute of Standards and Technology, Department of commerce, United States of America for Ca, Mn, Fe, Zn, Cu and the Standard Addition Methods for Pb. The accuracy of the Standard Addition Methods was estimated by CRM281 Rye Grass of Community Bureau of Reference-BCR, European Commission. The results of 10 samples which were collected from several markets in Hanoi are shown. (author)

  7. 100-OL-1 Operable Unit Field Portable X-Ray Fluorescence (XRF) Analyzer Pilot Study Plans

    Bunn, Amoret L.; Fritz, Brad G.; Wellman, Dawn M.

    2014-07-15

    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.

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

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

  9. Confocal X-ray fluorescence micro-spectroscopy experiment in tilted geometry

    This paper provides a generalized mathematical model to describe the intensity of primary X-ray fluorescence radiation collected in the tilted confocal geometry mode, where the collimating optics is rotated over an angle relative to a horizontal plane. The influence of newly introduced terms, which take into account the tilted geometry mode, is discussed. The model is verified with a multi-layer test sample scanned in depth. It is proved that for low-Z matrices, the rotation of the detection channel does not induce any significant differences in a reconstruction of the thickness and chemical composition of layers, so that it may safely be ignored. - Highlights: • A mathematical model for confocal XRF spectroscopy in tilted geometry was derived. • Tilted geometry influenced the analytical capabilities of XRF instrument slightly. • Thickness and the chemical composition of multi-layers were determined

  10. Multielement analysis of soils: a proposal involving a portable X-ray fluorescence equipment

    Juliana Terra

    2014-10-01

    Full Text Available Portable instruments are excellent choices to perform precision agriculture since they allow in situ information about soil composition. In such a way, results are obtained quickly and inputs can be applied promptly, depending on the local soil characteristics. This study aims to develop a method to measure inorganic elements at in natura soils using a portable EDXRF (Energy Dispersive X-ray Fluorescence equipment and multivariate calibration through Partial Least Square Regression (PLS. Seven certified reference standards are used to build the PLS models for Si, K, Ca, Mn and Fe. Two standards are separated for external PLS validation. Finally, the results show that a maximum of 21% is obtained for relative deviation.

  11. L shell X-ray fluorescence parameters of Pb in phthalocyanine complexes

    The L shell X-ray intensity ratios Li/Lα (i=l, β and γ), the production cross-sections σLi (i=l, α, β and γ) and the L3 subshell fluorescence yields ωL3 have been investigated for the element Pb in the phthalocyanine complexes. The measurements have been performed using an 241Am annular radioactive source and an Ultra-LEGe detector with a resolution of 150 eV at 5.9 keV. The experimental values have been compared with the theoretical values of pure Pb element. - Highlights: • The L shell XRF parameters of Pb in the phthalocyanine complexes were investigated. • These parameters were obtained using EDXRF method. • The results are agreement with the theoretical values

  12. Characterization of nuclear materials by total reflection X-ray fluorescence spectrometry

    Nuclear energy is one of the available energy options for long term energy security of world. In order to produce electricity using this mode of energy generation in an efficient and safe manner, it is necessary that the materials used for such energy generation comply with the specifications assigned. The major and trace composition of these materials is an important specification for their quality control. Different analytical techniques are used for such quality control. Total reflection X-ray fluorescence (TXRF) is a comparatively new technique having several features well suited for trace and major element determinations in nuclear materials. However, this technique has not been used so far extensively for characterization of nuclear materials. The present paper gives a brief introduction of TXRF, its suitability for nuclear material characterization and some details of the TXRF studies made in our laboratory for the characterization of nuclear materials. (author)

  13. Mapping metals in Parkinson's and normal brain using rapid-scanning x-ray fluorescence

    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.

  14. Mapping metals in Parkinson's and normal brain using rapid-scanning x-ray fluorescence

    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.

  15. X-Ray Fluorescence to Determine Zn in Bolivian Children using Hair Samples

    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. Analytic Comparison between X-ray Fluorescence CT and K-edge CT

    Feng, Peng; Cong, Wenxiang; Wei, Biao

    2013-01-01

    X-ray fluorescence computed tomography (XFCT) and K-edge computed tomography (CT) are two important modalities to quantify a distribution of gold nanoparticles (GNPs) in a small animal for preclinical studies. It is valuable to determine which modality is more efficient for a given application. In this paper, we report a theoretical analysis in terms of signal-to-noise ratio (SNR) for the two modalities, showing that there is a threshold for the GNPs concentration and XFCT has a better SNR than K-edge CT if GNPs concentration is less than this threshold. Numerical simulations are performed and two kinds of phantoms are used to represent multiple concentration levels and feature sizes. Experimental results illustrate that XFCT is superior to K-edge CT when contrast concentration is lower than 0.4% which coincides with the theoretical analysis.

  17. Exams for attribution of sevres porcelain by x-ray fluorescence in Havana museums

    Analysis with X-ray fluorescence on Sevres porcelain was performed in order to determine criteria from the scientific examination that may support the attribution of special pieces. Multielemental chemical analyses of decorations colours, marks and glazed porcelain body were related to specific historic information about used materials and procedure of Sevres french manufactory. The used portable XRF spectrometer allows non destructive and in situ studies of Havana's collections with adequate sensibility for this application. Collections of Havana City Museum, Decorative Art Museum and Napoleonic Museum and some pieces of different background were studied. Non typical pigments used in Sevres allows to identify non genuine Sevres decorations while cluster analysis on porcelain body differentiates Sevres and 'surdecor' porcelains from Sevres style non genuine porcelains. (author)

  18. Direct elemental analysis of cancer cell lines by total reflection X-ray fluorescence

    The elemental content of Cu, Fe and Zn in two human adenocarcinoma cell lines was investigated by total reflection X-ray fluorescence (TXRF) spectrometry. Cancer cells were sedimented directly to the quartz plates using a modified cytospin slide holder setup. Special glass stands and caps were also constructed to hold the quartz plates with the cells during the vapour-phase microwave assisted digestion. The method was validated by analysis of certified reference materials. The signal-to-noise ratio was optimized by washing the cells with different solutions. The technique was applied to the determination of Cu, Fe and Zn content of HT-29 and HCA-7 colorectal adenocarcinoma cell lines. Dry mass of the centrifuged cells were determined and the elemental analysis data reported for the two cell lines were referred either to cell numbers, to the total protein content or to the dry mass

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

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

    2005-07-01

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

  20. Noninvasive in vivo percutaneous absorption measurements using x-ray fluorescence

    A new, noninvasive method for determining percutaneous absorption in vivo has been developed using radioisotope induced X-ray fluorescence (XRF). The absorption rate of 5-iodouracil in dimethyl sulfoxide (DMSO) was determined on four female Sprague-Dawley albino rats. The technique has also been used to investigate the penetration enhancing effects of ethyl acetate (EtoAc), N-methyl 2-pyrrolidinone (NMP), and DMSO with 2-iodobenzoic acid as the model compound. Several absorption kinetics were observed; zero order for EtoAc, first order for NMP, and a two compartment model for DMSO. The advantage of this disappearance measurement over the traditional radiolabeling method is that XRF is a simple, economical method in which the subject receives only a localized, low radiation dose (8 mR/5 min)

  1. X-Ray Fluorescence to Determine Zn in Bolivian Children using Hair Samples

    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. [Centro de Investigaciones y Aplicaciones Nucleares (CIAN-Viacha), Viacha (Bolivia, Plurinational State of); Romero Bolaños, L.E. [Instituto Boliviano de Ciencia y Tecnología Nuclear Av. 6 de Agosto 2905, La Paz (Bolivia, Plurinational State of); Ramírez Ávila, G.M., E-mail: gramirez@ulb.ac.be [Instituto de Investigaciones Físicas, Universidad Mayor de San Andrés, Campus Universitario Cota Cota, Casilla 8635, La Paz (Bolivia, Plurinational State of)

    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.

  2. Study of the hydrogen peroxide bleaching agent effects on bovine enamel using X-ray fluorescence

    Hydrogen Peroxide's a bleaching agent capable of oxidizing a wide range of colored organic, causing discoloration and hence bleaching of the substrate, but some authors related the occurrence of side effects related to bleaching of the tooth structure, such as changes in morphology superficial. It was used 6 bovine incisors, each tooth was initially evaluated six times in different areas to obtain the count of elements phosphorus and calcium using X-Ray Fluorescence. The teeth were randomly divided in two groups: both groups were submitted to bleaching in office with hydrogen peroxide 38%, once a week during three weeks. Group 1 was stored in distilled water and group 2 in artificial saliva, between the sessions. The measurements were repeated every seven days before the bleaching treatment. Besides that, changes in mineral levels were always assessed in the same area and using the same procedure. It was observed that the bleaching was not able to demineralize the tooth enamel studied. (author)

  3. The determination of trace elements in uranium ores by x-ray fluorescence spectrometry

    The determination of 17 trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Rb, Sr, Th, U, V, Y, Zn and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated in this study. The determination of major elements was also necessary for the calculation of mass absorption coefficients. Initially a method was developed for the determination of the elements of interest in unmineralised silicates. Correction for absorption of radiation by the sample were made by means of mass absorption coefficients which were obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. The Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. It was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample

  4. Determination of impurities in magnesium and aluminium by X-ray fluorescence spectrometry

    The determination of traces of Al, Cr, Cu, Fe, Mn, Ni, Pb, Si and of Bi, Cr, Cu, Fe, Ga, Mg, Mn, Ni, Pb, Si, Sn, Ti, V and Zn in samples of magnesium and aluminium, respectively, by means of X-ray fluorescence spectrometry, are studied. An automatic sequential spectrometer with an on-line computer for the treatment of data has been employed. The most suitable measurement parameters have been chosen for each element in order to achieve detection limits to a few p.p.m. For magnesium in the form of drillings the analyses are performed with satisfactory results for most impurities by pressing the samples into briquettes and employing metallic discs as standards. Correction methods for the spectral interferences of Ti on V, and V on Cr have been applied. (author)

  5. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    Fernandez-Ruiz, R. [Universidad Autonoma de Madrid, Facultad de Ciencias, Servicio Interdepartamental de Investigacion, Modulo C-9, Laboratorio de TXRF, Crta. Colmenar, Km 15, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Garcia-Heras, M. [Instituto de Historia-CSIC, C/Serrano, 13. E-28001, Madrid (Spain); CENIM-CSIC, Avda. Gregorio del Amo, 8. E-28040, Madrid (Spain)

    2007-10-15

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications.

  6. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications

  7. [Determination of major elements in superphosphate by X-ray fluorescence spectrometry].

    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. PMID:19271522

  8. High resolution X-ray fluorescence imaging for a microbeam radiation therapy treatment planning system

    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.

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

    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. - Highlights: ► We determine heavy metals in hair sample of sanitation workers and control group. ► 7 heavy metals, Mn, Fe, Ni, Cu, Zn, Se, and Sb, were detected in both groups. ► Additional elements of As, Hg and Pb were discovered only in sanitation workers. ► Generally, mean concentration of sanitation workers show elevation in comparison. ► We report results in relation to their respective heavy metals concentrations.

  10. Uranium and plutonium solution assays by transmission-corrected x-ray fluorescence

    Ryon, R W; Ruhter, W D; Rudenko, V; Sirontinin, A; Petrov, A A

    1999-09-08

    We have refined and tested a previously developed x-ray fluorescence analysis technique for uranium and plutonium solutions that compensates for variations in the absorption of the exciting gamma rays and fluorescent x-rays. We use {sup 57}Co to efficiently excite the K lines of the elements, and a mixed {sup 57}Co plus {sup 153}Gd transmission source to correct for variations in absorption. The absorption correction is a unique feature of our technique. It is possible to accurately calibrate the system with a single solution standard. There does not need to be a close match in composition (i.e., absorption) between the standard(s) and solutions to be analyzed. Specially designed equipment incorporates a planar intrinsic germanium detector, excitation and transmission radioisotopes, and specimen holder. The apparatus can be inserted into a rubber glove of a glovebox, keeping the apparatus outside and the solutions inside the glovebox, thereby protecting the user and the equipment from possible contamination. An alternate design may be used in chemical reprocessing plants, providing continuous monitoring, by measuring the trans-actinides through stainless steel piping. This technique has been tested at the Bochvar Research Institute of Inorganic Materials in Moscow for possible use in the Russian complex of nuclear facilities. This is part of a cooperative program between laboratories in the United States and Russia to strengthen systems of nuclear materials protection, control, and accountability (MPC and A). A part of this program is to accurately measure and track inventories of materials, thus the need for good non-destructive analytical techniques such as the one described here.

  11. Identifying microbial habitats in soil using quantum dots and x-ray fluorescence microtomography

    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.

  12. Three approaches for direct analysis of biological samples by Total reflection X-Ray Fluorescence analysis

    One of the main advantages of the Total reflection X-Ray Fluorescence technique is feasibility of the direct analysis of the sample. taking in account this fact, three methods for the direct analysis of biological samples were evaluated For the evaluation of the method of Compton peak standardization serum, brain tissue, urine and amniotic fluid matrices were analyzed using compton Peak and the elements Co, and V as internal standard. In the case the sample itself is used as calibration standard. The method is reliable for the analysis of serum and brain tissue samples. The analytical quality of the results was similar to that obtained by the conventional method. The results were in good agreements with those obtained by the atomic absorption technique. The second method was applied to the certified Bovine Liver Standard sample 1577a. Experimental conditions for the microwave acid digestion of the solid sample directly on the quartz reflector were found, The percent of recovery of the elements S, Ci, K, Ca, Mn, Fe, Cu, Zn, Se, Br, and Rb carried between 85% and 115% and The precision was below the 10% of relative standards deviations for ten independent replicates. In the third method the concept of chemical modifications is adapted to the Total reflection X-Ray Fluorescence technique. In these experiments the main objective was the elimination of Chlorine from the matrix following the in situ addition of the reactive ammonium nitrate and heating. The method was applied to high saline content samples, i.e. amniotic fluid samples, Special care was given to the volatile elements and to the quality of the thin layer. an enhancement of the sensitivity was found for those elements with signals near the chlorine k-Alfa signal after the modifications procedure

  13. The design of the hazardous substance sorting system. Applicability check of X-ray fluorescence spectrometer

    Construction of LEDF (Large Equipment Dismantling Facility) is being planned by Waste Management Section. This purpose of LEDF is the melting treatment of the radioactive waste in OEC (O-arai Engineering Center) and the waste package in JAERI (O-arai Japan Atomic Energy Research Institute). It is also considered about the disposal plan of the future. Therefore LEDF has the sorting process of waste because of the removal of problematic substances. But that process is conducted using its human eyes. This process needs automatic operation because of high classification accuracy, high reliability, burden reduction of a worker. Then we select EXFS (Energy dispersive X-ray Fluorescence Spectrometer), and conducted the measurement of waste (a sample) with this device. That purpose is to confirm an application as the sorting device. A confirmation result is shown in the following. (1) Sorting performance. Measurement is possible without pretreatment, if it is metal. However, sorting is difficult when paint, plating, impurities, etc. are shown in the surface. (2) Measurement position. It is necessary to set a gap of the measurement thing from a measurement position to 4mm or less. (3) Radiation influence. Because the background had risen by the influence of a radiant ray, the distinction of Fluorescence X-ray became difficult. Therefore the distinction of materials became impossible. Aluminum is influenced specially by it. As a conclusion, the application nature of EXFS thing Sorting System is high. But there is a bad influence by radiation. Therefore, difficult is installation into the cell. In order to apply EXFS to LEDF, it is necessary to place it outside the cell and to use as the help of the visual inspection. (author)

  14. Elementary chemical analysis in leaves infected by fumagina by X-Ray fluorescence technique

    Maria Sélia Blonski

    2007-09-01

    Full Text Available Energy Dispersion X-Ray Fluorescence Technique (EDXRF was employed to study the effects of the fumagina disease on the elementary chemical composition of the leaves. The experimental set up consisted of a Mo X-ray tube (Ksubµ = 17.44 keV with Zr filter and a Si (Li detector. The measurements were performed with the infected and healthy leaves of citric plants. The elements Ti, Mn, Fe, Cu and Zn were quantified, with an average DL of 69, 12, 8, 4 and 4 µg.g-1 respectively. The obtained concentration for Fe varied from 44 to 192 µg.g-1 in healthy leaves and from 363 to 704 µg.g-1 in infected leaves with fumagina .Foi empregada a técnica de fluorescência de raios X por dispersão de energia (EDXRF, para estudar os efeitos da doença fumagina na composição química elementar de folhas. O arranjo experimental consistiu de um tubo de raios X com anodo de Mo (Kµ = 17.44 keV com filtro de Zr e um detector de Si(Li. As medidas foram realizadas com folhas de plantas cítricas infectadas e sadias. Foram quantificados os elementos Ti, Mn, Fe, Cu e Zn, com um limite de detecção médio de 69, 12, 8, 4 e 4 µg.g-1 respectivamente. As concentrações obtidas para o Fe variaram de 44 a 192 µg.g-1 em amostras de folhas sadias e de 363 a 704 µg g-1 para as folhas infectadas com fumagina.

  15. Quantitative micro x-ray fluorescence analyses without reference standard material; Referenzprobenfreie quantitative Mikro-Roentgenfluoreszenzanalyse

    Wolff, Timo

    2009-07-15

    X-ray fluorescence analysis (XRF) is a standard method for non-destructive investigations. Due to the development of polycapillary optics and SDDdetectors requiring no cooling with liquid nitrogen, XRF becomes a suitable method for a large number of applications, e. g. for the analysis of objects in arts and archaeology. Spectrometers developed for those purposes allow investigations outside of laboratories und provide excitation areas with diameters of 10-70 {mu}m. In most applications, quantification of XRF data is realized by the usage of standard reference materials. Due to absorption processes in the samples the accuracy of the results depends strongly on the similarity of the sample and the reference standard. In cases where no suitable references are available, quantification can be done based on the ''fundamental parameter (fp) method''. This quantification procedure is based on a set of equations describing the fluorescence production and detection mathematical. The cross sections for the interaction of x-rays with matter can be taken from different databases. During an iteration process the element concentrations can be determined. Quantitative XRF based on fundamental parameters requires an accurate knowledge of the excitation spectrum. In case of a conventional setup this spectrum is given by the X-ray tube spectrum and can be calculated. The use of polycapillary optics in micro-XRF spectrometers changes the spectral distribution of the excitation radiation. For this reason it is necessary to access the transmission function of the used optic. The aim of this work is to find a procedure to describe this function for routine quantification based on fundamental parameters. Most of the measurements have been carried out using a commercial spectrometer developed for applications in arts and archaeology. On the one hand the parameters of the lens, used in the spectrometer, have been investigated by different experimental characterization

  16. Synchrotron X-ray fluorescence studies of a bromine-labelled cyclic RGD peptide interacting with individual tumor cells

    The first example of synchrotron X-ray fluorescence imaging of cultured mammalian cells in cyclic peptide research is reported. The study reports the first quantitative analysis of the incorporation of a bromine-labelled cyclic RGD peptide and its effects on the biodistribution of endogenous elements (for example, K and Cl) within individual tumor cells. The first example of synchrotron X-ray fluorescence imaging of cultured mammalian cells in cyclic peptide research is reported. The study reports the first quantitative analysis of the incorporation of a bromine-labelled cyclic RGD peptide and its effects on the biodistribution of endogenous elements (for example, K and Cl) within individual tumor cells

  17. Determination of niobium content in Zr-Nb alloys by Wavelength Dispersive X-ray Fluorescence Spectrometry

    Quantitative determination of niobium content in zirconium alloys, viz. Zr-2.5% Nb and Zr-1% Nb by Wavelength Dispersive X-Ray Fluorescence Spectrometer (WDXRFS) has been described in the paper. The results are compared with those obtained by Direct Reading Emission Spectrometer (DRES) for Zr-2.5%Nb samples. For Zr-1%Nb samples, analysis by wavelength dispersive x-ray fluorescence spectrometry in two modes viz. through solution mode and by nondestructive solid sample analysis were performed and the results are compared. A RSD of < 1% is obtained in the technique. (author)

  18. 2D/3D cryo x-ray fluorescence imaging at the bionanoprobe at the advanced photon source

    Chen, S., E-mail: sichen@aps.anl.gov; Vine, D. J.; Lai, B. [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Paunesku, T.; Yuan, Y.; Woloschak, G. E. [Department of Radiation Oncology, Northwester University, Chicago, IL 60611 (United States); Deng, J. [Applied Physics, Northwestern University, Evanston, IL 60208 (United States); Jin, Q.; Hong, Y. P. [Department of Physics and Astronomy, Northwestern University, Evanston, IL 60208 (United States); Flachenecker, C.; Hornberger, B. [Carl Zeiss X-ray Microscopy, Pleasanton, CA 94588 (United States); Brister, K. [Synchrotron Research Center, Northwestern University, Argonne, IL 60439 (United States); Jacobsen, C. [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Applied Physics, Northwestern University, Evanston, IL 60208 (United States); Department of Physics and Astronomy, Northwestern University, Evanston, IL 60208 (United States); Chemistry of Life Processes Institute, Northwestern University, Evanston, IL 60208 (United States); Vogt, S. [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Department of Radiation Oncology, Northwester University, Chicago, IL 60611 (United States)

    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.

  19. [Energy-dispersive x-ray fluorescence spectrometry--a forensic chemistry method for determination of shooting distance].

    Havel, J

    2003-10-01

    The article follows up the experiences Energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic necrochemical method as the tool for detection of metals (gunshot residues--GSR) in connection with gunshot-wounds of persons--authors: dipl. Ing. J. Havel and dipl. Ing. K. Zelenka and Energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic method as the tool for identification of inlets (gunshot--entries) and outlets (gunshot--exits)--author: dipl. Ing. J. Havel. PMID:14661530

  20. Portable and micro x-ray fluorescence investigations of the wall paintings belonging to different periods of anatolian history

    Full text: In this study portable x-ray fluorescence spectrometer and micro x-ray fluorescence spectrometer were used for investigating the pigments on the Chatalhoyuk wall paintings from the neolithic period which are located in Museum of Anatolian Civilizations. Totally 15 artifacts were investigated in this study and the elemental compositions of the pigments were identified on this paintings. The communities which have lived in different periods of time have revealed different cultures during the 12 000 years old cultural heritage in our country