WorldWideScience

Sample records for 3d-micro x-ray fluorescence

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

    DEFF Research Database (Denmark)

    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......-XRF set-up is suitable for dating of minerals with low Pb concentrations as long as all Pb is radiogenic, allowing spatial resolution comparable to ion microprobe or laser ablation techniques. The set-up was tested on monazites that are well characterized by isotopic techniques and have a wide range...... of 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...

  2. X-ray Fluorescence Sectioning

    CERN Document Server

    Cong, Wenxiang

    2012-01-01

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

  3. X-ray fluorescence holography

    CERN Document Server

    Hayashi, K; Takahashi, Y

    2003-01-01

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

  4. Filtered fluorescer x-ray detector

    Energy Technology Data Exchange (ETDEWEB)

    Bruns, H.C.; Emig, J.A.; Thoe, R.S.; Springer, P.T.; Hernandez, J.A.

    1995-04-01

    Recently, an instrument capable of measuring x-rays between 8 and 90 keV was conceived to help understand conditions pertaining to pulsed power research. This resulted in the development of a versatile device that would incrementally detect x-rays emitted at predetermined energy bands over this range. To accomplish this, an array of well characterized filter-fluorescer combinations were produced which would allow fluoresced x-rays to be observed by time resolved electro-optical devices. As many as sixteen channels could be utilized with each channel having a corresponding background channel. Upon completion of the device, a three week series of experiments was then successfully carried out.

  5. Ex-situ time-lapse x-ray CT study of 3D micro-structural fatigue damage evolution in uni-directional composites

    DEFF Research Database (Denmark)

    Jespersen, Kristine Munk; Wang, Ying; Zangenberg Hansen, Jens

    2016-01-01

    In this study, the progress of damage under tension-tension fatigue of a uni-directional (UD) glass fibre composite made from a non-crimp fabric is studied using transilluminated white light imaging (TWLI) and X-ray computed tomography (CT). TWLI images are automatically captured throughout...

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

    Institute of Scientific and Technical Information of China (English)

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

    2011-01-01

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

  7. Surface-Enhanced X-Ray Fluorescence

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  9. A Monte Carlo study of x-ray fluorescence in x-ray detectors.

    Science.gov (United States)

    Boone, J M; Seibert, J A; Sabol, J M; Tecotzky, M

    1999-06-01

    Advances in digital x-ray detector systems have led to a renewed interest in the performance of x-ray phosphors and other detector materials. Indirect flat panel x-ray detector and charged coupled device (CCD) systems require a more technologically challenging geometry, whereby the x-ray beam is incident on the front side of the scintillator, and the light produced must diffuse to the back surface of the screen to reach the photoreceptor. Direct detector systems based on selenium have also enjoyed a growing interest, both commercially and academically. Monte Carlo simulation techniques were used to study the x-ray scattering (Rayleigh and Compton) and the more prevalent x-ray fluorescence properties of seven different x-ray detector materials, Gd2O2S, CsI, Se, BaFBr, YTaO4, CaWO4, and ThO2. The redistribution of x-ray energy, back towards the x-ray source, in a forward direction through the detector, and lateral reabsorption in the detector was computed under monoenergetic conditions (1 keV to 130 keV by 1 keV intervals) with five detector thicknesses, 30, 60, 90, 120, and 150 mg/cm2 (Se was studied from 30 to 1000 mg/cm2). The radial distribution (related to the point spread function) of reabsorbed x-ray energy was also determined. Representative results are as follows: At 55 keV, more (31.3%) of the incident x-ray energy escaped from a 90 mg/cm2Gd2O2S detector than was absorbed (27.9%). Approximately 1% of the total absorbed energy was reabsorbed greater than 0.5 mm from the primary interaction, for 90 mg/cm2 CsI exposed at 100 kVp. The ratio of reabsorbed secondary (fluorescence + scatter) radiation to the primary radiation absorbed in the detectors (90 mg/cm2) (S/P) was determined as 10%, 16%, 2%, 12%, 3%, 3%, and 0.3% for a 100 kVp tungsten anode x-ray spectrum, for the Gd2O2S, CsI, Se, BaFBr, YTaO4, CaWO4, and ThO2 detectors, respectively. The results indicate significant x-ray fluorescent escape and reabsorption in common x-ray detectors. These findings

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    CERN Document Server

    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.

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

    OpenAIRE

    Lane, D W.; 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...

  13. Milli X-Ray Fluorescence Spectrometer

    Data.gov (United States)

    Federal Laboratory Consortium — The Eagle III Micro XRF unit is similar to a traditional XRF unit, with the primary difference being that the X-rays are focused by a polycapillary optic into a spot...

  14. High-Definition X-Ray Fluorescence: Applications

    OpenAIRE

    Gibson, Walter M.; Chen, Z W; Li, Danhong

    2008-01-01

    Energy dispersive X-ray fluorescence (EDXRF) is a well-established and powerful tool for nondestructive elemental analysis of virtually any material. It is widely used for environmental, industrial, pharmaceutical, forensic, and scientific research applications to measure the concentration of elemental constituents or contaminants. The fluorescing atoms can be excited by energetic electrons, ions, or photons. A particular EDXRF method, monochromatic microbeam X-ray fluorescence (MμEDXRF), has...

  15. High Definition X-Ray Fluorescence: Principles and Techniques

    OpenAIRE

    Chen, Z W; Gibson, Walter M.; Huang, Huapeng

    2008-01-01

    Energy dispersive X-ray fluorescence (EDXRF) is a well-established and powerful tool for nondestructive elemental analysis of virtually any material. It is widely used for environmental, industrial, pharmaceutical, forensic, and scientific research applications to measure the concentration of elemental constituents or contaminants. The fluorescing atoms can be excited by energetic electrons, ions, or photons. A particular EDXRF method, monochromatic microfocus X-ray fluorescence (MμEDXRF), ha...

  16. X-ray Fluorescent Fe Kalpha Lines from Stellar Photospheres

    CERN Document Server

    Drake, Jeremy J; Swartz, Douglas A

    2007-01-01

    X-ray spectra from stellar coronae are reprocessed by the underlying photosphere through scattering and photoionization events. While reprocessed X-ray spectra reaching a distant observer are at a flux level of only a few percent of that of the corona itself, characteristic lines formed by inner shell photoionization of some abundant elements can be significantly stronger. The emergent photospheric spectra are sensitive to the distance and location of the fluorescing radiation and can provide diagnostics of coronal geometry and abundance. Here we present Monte Carlo simulations of the photospheric Kalpha doublet arising from quasi-neutral Fe irradiated by a coronal X-ray source. Fluorescent line strengths have been computed as a function of the height of the radiation source, the temperature of the ionising X-ray spectrum, and the viewing angle. We also illustrate how the fluorescence efficiencies scale with the photospheric metallicity and the Fe abundance. Based on the results we make three comments: (1) fl...

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

    Energy Technology Data Exchange (ETDEWEB)

    Miller, Thomasin C. [X-ray Optical Systems, Inc., East Greenbush, NY 12180 (United States)]. E-mail: tmiller@xos.com; Langley DeWitt, Helen [Chemistry Division, Analytical Chemistry Science, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Havrilla, George J. [Chemistry Division, Analytical Chemistry Science, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2005-11-15

    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 Dot{sup TM} 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 {approx} 0.04 ng and a mean particle diameter of {approx} 0.06 {mu}m. 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.

  18. Resonant soft X-ray fluorescence spectra of molecules

    Energy Technology Data Exchange (ETDEWEB)

    Nordgren, J.; Glans, P.; Gunnelin, K.; Guo, J.; Skytt, P.; Saathe, C.; Wassdahl, N. [Uppsala Univ. (Sweden). Dept. of Phys.

    1997-08-01

    A review is presented of some recent advancements in resonant soft X-ray fluorescence spectroscopy applied to molecules. The concept of inelastic scattering is discussed for molecules with an element of symmetry, which introduces degeneracy or near-degeneracy of core excited states. The potential of the symmetry selection rules associated with resonant X-ray fluorescence is illustrated in studies of electronic structure as well as molecular dynamics. The use of polarized photons for exciting X-ray emission is discussed, and examples are presented where anisotropy of X-ray emission provides more detailed information. A brief section discusses the experimental considerations relevant for the spectroscopic technique. (orig.) With 013 figs., 28 refs.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    1999-01-01

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

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

    Science.gov (United States)

    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.

  2. HIgh Rate X-ray Fluorescence Detector

    Energy Technology Data Exchange (ETDEWEB)

    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

    Science.gov (United States)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  4. X-ray fluorescence microscopy of olfactory receptor neurons

    Energy Technology Data Exchange (ETDEWEB)

    Ducic, T; Herbst, J; Novakova, E; Salditt, T [Institute for X-ray Physics, Georg-August-University, Friedrich-Hund-Pl. 1, 37077 Goettingen (Germany); Breunig, E; Schild, D [Department of Molecular Neurophysiology, Georg-August University Goettingen (Germany); Susini, J; Tucoulu, R, E-mail: tducic@gwdg.d [European Synchrotron Radiation Facility ESRF, 6 rue Jules Horowitz, 38043 Grenoble (France)

    2009-09-01

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

  5. Submicron hard X-ray fluorescence imaging of synthetic elements

    Energy Technology Data Exchange (ETDEWEB)

    Jensen, Mark P., E-mail: mjensen@anl.gov [Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Aryal, Baikuntha P. [Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Department of Chemistry, University of Chicago, Chicago, IL 60637 (United States); Gorman-Lewis, Drew [Chemical Sciences and Engineering Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Paunesku, Tatjana [Department of Radiation Oncology, Feinberg School of Medicine, Northwestern University, Chicago, IL 60611 (United States); Department of Radiology, Feinberg School of Medicine, Northwestern University, Chicago, IL 60611 (United States); Lai, Barry; Vogt, Stefan [X-ray Science Division, Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); Woloschak, Gayle E. [Department of Radiation Oncology, Feinberg School of Medicine, Northwestern University, Chicago, IL 60611 (United States); Department of Radiology, Feinberg School of Medicine, Northwestern University, Chicago, IL 60611 (United States)

    2012-04-13

    Highlights: Black-Right-Pointing-Pointer Actinide elements are mapped with L-edge X-rays and better than 400 nm resolution. Black-Right-Pointing-Pointer A typical detection limit was 2.9 Multiplication-Sign 10{sup -20} moles Pu {mu}m{sup -2}. Black-Right-Pointing-Pointer XANES measurements provide chemical information in 0.1 {mu}m{sup 2} spots. Black-Right-Pointing-Pointer Selection of materials for encapsulation is important for avoiding interferences. - Abstract: Synchrotron-based X-ray fluorescence microscopy (XFM) using hard X-rays focused into sub-micron spots is a powerful technique for elemental quantification and mapping, as well as microspectroscopic measurements such as {mu}-XANES (X-ray absorption near edge structure). We have used XFM to image and simultaneously quantify the transuranic element plutonium at the L{sub 3} or L{sub 2}-edge as well as Th and lighter biologically essential elements in individual rat pheochromocytoma (PC12) cells after exposure to the long-lived plutonium isotope {sup 242}Pu. Elemental maps demonstrate that plutonium localizes principally in the cytoplasm of the cells and avoids the cell nucleus, which is marked by the highest concentrations of phosphorus and zinc, under the conditions of our experiments. The minimum detection limit under typical acquisition conditions with an incident X-ray energy of 18 keV for an average 202 {mu}m{sup 2} cell is 1.4 fg Pu or 2.9 Multiplication-Sign 10{sup -20} moles Pu {mu}m{sup -2}, which is similar to the detection limit of K-edge XFM of transition metals at 10 keV. Copper electron microscopy grids were used to avoid interference from gold X-ray emissions, but traces of strontium present in naturally occurring calcium can still interfere with plutonium detection using its L{sub {alpha}} X-ray emission.

  6. Portable energy dispersive X-ray fluorescence and X-ray diffraction and radiography system for archaeometry

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza Cuevas, Ariadna, E-mail: ariadna@mail.or [Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana, Obispo, entre San Ignacio y Mercaderes, Habana Vieja, cp 10 100, Havana (Cuba); Perez Gravie, Homero, E-mail: homero.perezgravie@mail.co [Archaeometry Laboratory, Colegio Universitario San Geronimo de La Habana, Obispo, entre San Ignacio y Mercaderes, Habana Vieja, cp 10 100, Havana (Cuba)

    2011-03-21

    Starting on a laboratory developed portable X-ray fluorescence (PXRF) spectrometer; three different analytical results can be performed: analysis of chemical elements, analysis of major chemical crystalline phase and structural analysis, which represents a contribution to a new, low cost development of portable X-ray analyzer; since these results are respectively obtained with independent equipments for X-ray fluorescence, X-ray diffraction and radiography. Detection limits of PXRF were characterized using standard reference materials for ceramics, glass, bronze and bones, which are the main materials requiring quantitative analysis in art and archeological objects. A setup for simultaneous energy dispersive X-ray fluorescence and diffraction (ED (XRF-XRD)) in the reflection mode has been tested for in situ and non-destructive analysis according to the requirements of art objects inspection. The system uses a single low power X-ray tube and an X-ray energy dispersive detector to measure X-ray diffraction spectrum at a fixed angle. Application to the identification of jadeite-jade mineral in archeological objects by XRD is presented. A local high resolution radiography image obtained with the same low power X-ray tube allows for studies in painting and archeological bones.

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

    Science.gov (United States)

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

    2016-10-01

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

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  10. Proton-induced x-ray fluorescence CT imaging

    Energy Technology Data Exchange (ETDEWEB)

    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

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

    Science.gov (United States)

    Groover, Krishangi D.; Izbicki, John

    2016-06-24

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

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

    Science.gov (United States)

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

    2012-01-01

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

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

    Science.gov (United States)

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

    2012-01-01

    Procedures for preparation of Lauha Bhasma are described in ancient texts of Ayurveda. These procedures also begin with different source material for iron such as Teekshna Lauha and Kanta Lauha etc. In the present study, we have selected different source materials viz. magnetite iron ore for Kanta Lauha and pure (Armco grade) iron turnings for Teekshna Lauha. The standard procedures of preparation of Lauha Bhasma are carried out in identical conditions for these two raw materials. The final product from the Puta are characterized by using X-ray diffraction and X-ray fluorescence spectroscopy to understanding the crystallographic form or forms of iron oxides and their composition at the end of each Puta. The iron content at the end of repeated Putas (18 for Kanta Lauha and 20 for Teekshna Lauha) have shown a decrease in case of Teekshna Lauha since the starting material is pure iron while it showed only marginal decreases in the case of Kanta Lauha because the Fe3O4 of magnetite is undergoing oxidation to Fe2O3. The trace elements remain within the Bhasma in the form of various oxides of Si, Al, Ca, etc. PMID:23049200

  14. Trends in environmental science using microscopic X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, Ursula Elisabeth Adriane, E-mail: ursula.fittschen@chemie.uni-hamburg.de [Department of Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Falkenberg, Gerald [Deutsches Elektronen-Synchrotron, Notkestr. 85, 22603 Hamburg (Germany)

    2011-08-15

    Microscopic X-ray fluorescence (micro-XRF) is a versatile tool in environmental analysis. We review work done in this field from 2008 to 2010 and highlight new aspects. Overall, there is a strong trend to combine fluorescence data with other data like diffraction or absorption spectroscopy. Also, the use of laboratory based instrumentation has become wide spread as more commercial instruments are available. At laboratories and synchrotron sites the trend towards higher spatial resolution is still persistent hitting sub micrometer values in case of synchrotron set ups.

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

    Energy Technology Data Exchange (ETDEWEB)

    Loupilov, A. E-mail: bsi@bsi.lv; Sokolov, A.; Gostilo, V

    2001-06-01

    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 mm{sup 2}, thickness=3.5 mm, 175 eV (5.9 keV), 430 eV (59.6 keV); S=100 mm{sup 2}; thickness=4.5 mm, 270 eV (5.9 keV), 485 eV (59.6 keV). (2.) Si-planar detector: S=10 mm{sup 2}, thickness=0.4 mm, 230 eV (5.9 keV), 460 eV (59.6 keV). (3.) CdTe p-i-n detectors: S=16 mm{sup 2}, thickness=0.5 mm, 350 eV (5.9 keV), 585 eV (59.6 keV). S=16 mm{sup 2}, 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, cryminalistics and history of art are demonstrated.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-11

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

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

    Science.gov (United States)

    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.

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

    Data.gov (United States)

    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...

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

    Data.gov (United States)

    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,...

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

    Energy Technology Data Exchange (ETDEWEB)

    Chwiej, Joanna [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland)]. E-mail: jchwiej@novell.ftj.agh.edu.pl; Szczerbowska-Boruchowska, Magdalena [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Lankosz, Marek [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Wojcik, Slawomir [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Falkenberg, Gerald [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron, Notkestr. 85, Hamburg (Germany); Stegowski, Zdzislaw [Faculty of Physics and Applied Computer Science, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Setkowicz, Zuzanna [Department of Neuroanatomy, Institute of Zoology, Jagiellonian University, Ingardena 6, 30-060 Cracow (Poland)

    2005-12-15

    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.

  1. Determination of beryllium by using X-ray fluorescence spectrometry.

    Science.gov (United States)

    Zawisza, Beata

    2008-03-01

    X-ray fluorescence spectrometry method is subject to certain difficulties and inconveniences for the elements having the atomic number 9 or less. These difficulties become progressively more severe as the atomic number decreases, and are quite serious for beryllium, which is practically indeterminable directly by XRF. Therefore, an indirect determination of beryllium that is based on the evaluation of cobalt in the precipitate is taken into consideration. In the thesis below, there is a description of a new, simple, and precise method by selective precipitation using hexamminecobalt(III) chloride and ammonium carbonate-EDTA solution as a complexing agent for the determining of a trace amount of beryllium using X-ray fluorescence spectrometry. The optimum conditions for [Co(NH(3))(6)][Be(2)(OH)(3)(CO(3))(2)(H(2)O)(2)].(3)H(2)O complex formation were studied. The complex was collected on the membrane filter, and the Co Kalpha line was measured by XRF. The method presents the advantages of the sample preparation and the elimination of the matrix effects due to the thin film obtained. The detection limit of the proposed method is 0.2 mg of beryllium. The method was successfully applied to beryllium determination in copper/ beryllium/cobalt alloys.

  2. Feasibility of x ray fluorescence for spent fuel safeguards

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, Corey Ross [Los Alamos National Laboratory; Mozin, Vladimir [Los Alamos National Laboratory; Tobin, Stephen J [Los Alamos National Laboratory; Fensin, Michael L [Los Alamos National Laboratory; White, Julia M [Los Alamos National Laboratory; Croft, Stephen [Los Alamos National Laboratory; Stafford, Alissa [TAMU; Charlton, William [TAMU

    2010-01-01

    Quantifying the Pu content in spent nuclear fuel is necessary for many reasons, in particular to verify that diversion or other illicit activities have not occurred. Therefore, safeguarding the world's nuclear fuel is paramount to responsible nuclear regulation and public acceptance, but achieving this goal presents many difficulties from both a technical and economic perspective. The Next Generation Safeguards Initiative (NGSI) of NA-24 is funding a large collaborative effort between multiple laboratories and universities to improve spent nuclear fuel safeguards methods and equipment. This effort involves the current work of modeling several different nondestructive assay (NDA) techniques. Several are being researched, because no single NDA technique, in isolation, has the potential to properly characterize fuel assemblies and offer a robust safeguards measure. The insights gained from this research, will be used to down-select from the original set a few of the most promising techniques that complement each other. The goal is to integrate the selected instruments to create an accurate measurement system for fuel verification that is also robust enough to detect diversions. These instruments will be fabricated and tested under realistic conditions. This work examines one of the NDA techniques; the feasibility of using x ray emission peaks from Pu and U to gather information about their relative quantities in the spent fuel. X Ray Fluorescence (XRF), is unique compared to the investigated techniques in that it is the only one able to give the elemental ratio of Pu to U, allowing the possibility of a Pu gram quantity for the assembly to be calculated. XRF also presents many challenges, mainly its low penetration, since the low energy x rays of interest are effectively shielded by the first few millimeters of a fuel pin. This paper will explore the results of Monte Carlo N-Particle eXtended (MCNPX) transport code calculations of spent fuel x ray peaks. The MCNPX

  3. X-ray fluorescence in research on Czech cultural monuments

    Energy Technology Data Exchange (ETDEWEB)

    Cechak, T.; Gerndt, J.; Kopecka, I.; Musilek, L. E-mail: musilek@fjfi.cvut.cz

    2004-01-01

    Radionuclide X-ray fluorescence analysis (RXRFA), as a non-destructive method, relatively simple and allowing measurements to be carried out in situ, is an excellent tool in research on various objects of art. A range of artefacts have been investigated by our laboratory, in part for the purposes of history of art and in part as a basis for restoration works - medieval frescoes in some Czech castles and churches, metal sculptures and objects of applied art, paints and inks of old manuscripts, paintings. Some of these are among the most valuable monuments in the Czech cultural heritage. The contribution of the results of the tests to the investigation of their 'life story' and, in some cases, to their conservation, is not negligible. Later additions and repairs can be recognised, and materials and technologies that are close to their historic counterparts can be used in restoration work.

  4. Promising X-ray fluorescence tests for superconducting tunneljunction detector

    Energy Technology Data Exchange (ETDEWEB)

    Friedrich, Stephan; Robinson, Arthur L.

    2001-05-15

    Scientists in the Physical Biosciences Division of the Ernest Orlando Berkeley National Laboratory (Berkeley Lab) studying transition metals in proteins with fluorescence-detected L-edge absorption spectroscopy have found the measurements to be extremely challenging. The difficulty is that the metal centers are present in very dilute concentrations so that their weak fluorescence is often obscured by strong background signals carbon and oxygen. To solve this problem, the Berkeley group has been working with researchers from the Advanced Detector Group at the Lawrence Livermore National Laboratory on an energy-dispersive superconducting tunnel junction x-ray detector. These devices in principle have the energy resolution needed to reveal the metal signal. The most recent results with the latest version of the detector on Beamline 4.0.1-2 at the Advanced Light Source (ALS) illustrate the promise of the cryogenic detector strategy not only for this application but also for spectroscopy of other types of dilute samples. Transition-metal complexes are key elements in many biologically important processes that are catalyzed by proteins (enzymes), photosynthesis being a prime example. The changes in that occur in electronic structure throughout a catalytic cycle are the subject of much research aimed at understanding the mechanisms of these processes. L-edge x-ray spectroscopy offers several advantages relative to the more common K-edge techniques, since it involves allowed transitions to the d-orbitals associated with metal-ligand bonding. It also has a rich multiplet structure interpretable by theory and higher spectral resolution.

  5. Materials characterization using micro-x-ray fluorescence elemental imaging.

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, G. J. (George J.); Miller, T. C. (Thomasin C.); Joseph, M. R. (Martha R.)

    2002-01-01

    Materials characterization continues to be a key challenge in a variety of programs. Although bulk elemental composition provides overall concentration of both major and trace elements, the distribution of these elements both on micro and macro scales can determine the performance and ultimately the physical properties of the materials. Hence elemental imaging can provide a new level of information for major and in some cases bulk trace concentrations of elements. Micro X-ray fluorescence (MXRF) offers unique capabilities in terms of elemental imaging. This approach is based on a meso scale level of resolution around 50 micrometer X-ray spot size. When coupled with a moveable stage, specimens several inches on a side can be imaged with surprising detail. In most instances, qualitative images are sufficient to illustrate the elemental heterogeneity. This information can then be used to determine if the material meets the desired physical characteristics and whether this is due to the observed heterogeneity or in spite of it. Several examples of elemental imaging will be presented. These will include the aging of polymers and the effects of residual organotin catalyst. The tin can be imaged using MXRF and has been show to be mobile within the polymeric material over time. Corrosion is a serious issue throughout the industrial world. A specific example of chloride attack on a metal, which creates problems in waste storage. Finally, MXRF used in high throughput screening in the development of novel peptide receptors will be shown. The advantage of MXRF is that no fluorescent tags need be added to the target molecules. This insures the unhindered interaction of the target molecules and allows for additional characterization using molecular spectroscopic techniques.

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-04-26

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    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.

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

    Science.gov (United States)

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

    2013-06-01

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

  10. X-ray Fluorescence Measurements of Turbulent Methane-Oxygen Shear Coaxial Flames (Briefing Charts)

    Science.gov (United States)

    2015-03-01

    Briefing Charts 3. DATES COVERED (From - To) March 2015-May 2015 4. TITLE AND SUBTITLE X-ray Fluorescence Measurements of Turbulent Methane -Oxygen Shear...1 DISTRIBUTION A: Approved for public release; distribution unlimited. Clearance # X-ray Fluorescence Measurements of Turbulent Methane -Oxygen Shear

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

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-12-01

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

  12. Water analysis via portable X-ray fluorescence spectrometry

    Science.gov (United States)

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

    2017-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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

  14. Feasibility study of total reflection X-ray fluorescence analysis using a liquid metal jet X-ray tube

    Energy Technology Data Exchange (ETDEWEB)

    Maderitsch, A.; Smolek, S. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria); Wobrauschek, P., E-mail: wobi@ati.ac.at [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria); Streli, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria); Takman, P. [Excillum AB, Finlandsgatan 14, 164 74 Kista (Sweden)

    2014-09-01

    Total reflection X-ray spectroscopy (TXRF) is a powerful analytical technique for qualitative and quantitative analysis of trace and ultratrace elements in a sample with lower limits of detection (LLDs) of pg/g to ng/g in concentration and absolute high fg levels are attainable. Several X-ray sources, from low power (few W), 18 kW rotating anodes to synchrotron radiation, are in use for the excitation and lead accordingly to their photon flux delivered on the sample the detection limits specified. Not only the power, but also the brilliance and focal shape are of importance for TXRF. A microfocus of 50–100 μm spot size or the line focus of diffraction tubes is best suited. Excillum developed a new approach in the design of a source: the liquid metal jet anode. In this paper the results achieved with this source are described. A versatile TXRF spectrometer with vacuum chamber designed at Atominstitut was used for the experiments. A multilayer monochromator selecting the intensive Ga-Kα radiation was taken and the beam was collimated by 50 μm slits. Excellent results regarding geometric beam stability, high fluorescence intensities and low background were achieved leading to detection limits in the high fg range for Ni. A 100 mm{sup 2} silicon drift detector (SDD) collimated to 80 mm{sup 2} was used to collect the fluorescence radiation. The results from measurements on single element samples are presented. - Highlights: • Using a new X-ray source for TXRF • Liquid metal jet X-ray source from Excillum • Offers improvements for lab based TXRF spectrometers • Can also be important for related techniques.

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

    Science.gov (United States)

    Cho, H-M; Ding, H; Ziemer, B P; Molloi, S

    2014-12-07

    Accurate energy calibration is critical for the application of energy-resolved photon-counting detectors in spectral imaging. The aim of this study is to investigate the feasibility of energy response calibration and characterization of a photon-counting detector using x-ray fluorescence. A comprehensive Monte Carlo simulation study was performed using Geant4 Application for Tomographic Emission (GATE) to investigate the optimal technique for x-ray fluorescence calibration. Simulations were conducted using a 100 kVp tungsten-anode spectra with 2.7 mm Al filter for a single pixel cadmium telluride (CdTe) detector with 3 × 3 mm(2) in detection area. The angular dependence of x-ray fluorescence and scatter background was investigated by varying the detection angle from 20° to 170° with respect to the beam direction. The effects of the detector material, shape, and size on the recorded x-ray fluorescence were investigated. The fluorescent material size effect was considered with and without the container for the fluorescent material. In order to provide validation for the simulation result, the angular dependence of x-ray fluorescence from five fluorescent materials was experimentally measured using a spectrometer. Finally, eleven of the fluorescent materials were used for energy calibration of a CZT-based photon-counting detector. The optimal detection angle was determined to be approximately at 120° with respect to the beam direction, which showed the highest fluorescence to scatter ratio (FSR) with a weak dependence on the fluorescent material size. The feasibility of x-ray fluorescence for energy calibration of photon-counting detectors in the diagnostic x-ray energy range was verified by successfully calibrating the energy response of a CZT-based photon-counting detector. The results of this study can be used as a guideline to implement the x-ray fluorescence calibration method for photon-counting detectors in a typical imaging laboratory.

  16. Study of Multi Total Reflection X-ray Fluorescence Spectrometer

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    A total reflection X-ray spectrometer was set up, in which Mo tube was used as excitation source, Zr with the thickness of 100 μm was as filter, and λ/20 glabrous silicon was as reflector, λ/100 glabrous silicon was as sample carrier.

  17. Research on U,Np,Pu Excitation Parameter With X-ray Fluorescence Analysis

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    <正>X-ray fluorescence analysis is a characteristic analysis technique widely applied in the geology environment and chemical industry. It is also an important quality control analytical method in nuclear

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

    Science.gov (United States)

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

    1996-01-01

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

  19. ISS Ammonia Leak Detection Through X-Ray Fluorescence

    Science.gov (United States)

    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

  20. Development of low-energy x-ray fluorescence micro-distribution analysis using a laser plasma x-ray source and multilayer optics?

    NARCIS (Netherlands)

    Stuik, R.; Shmaenok, L. A.; Fledderus, H.; Andreev, S. S.; Shamov, E. A.; Zuev, S. Y.; Salashchenko, N. N.; F. Bijkerk,

    1999-01-01

    A new technique is presented for low-energy X-ray fluorescence micro-distribution analysis of low-Z elements at micrometer spatial resolutions. The technique is based on the use of a laser plasma X-ray source and spherically curved multilayer optics. A large collimator is used to focus the light fro

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

    Science.gov (United States)

    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.

  2. Project Title: Radiochemical Analysis by High Sensitivity Dual-Optic Micro X-ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, George J.; Gao, Ning

    2003-06-01

    A novel dual-optic micro X-ray fluorescence instrument will be developed to do radiochemical analysis of high-level radioactive wastes at DOE sites such as Savannah River Site and Hanford. This concept incorporates new X-ray optical elements such as monolithic polycapillaries, which focus X-rays. The polycapillary optic can be used to focus X-rays emitted by the X-ray tube thereby increasing the X-ray flux on the sample over 1000 times. The polycapillary optic will also be used to collect the X-rays from the excitation site. This will effectively screen the radiation background from the radioactive species in the specimen. This dual-optic approach significantly reduces the background and increases the analyte signal thereby increasing the sensitivity of the analysis. This dual-capillary design is essentially a confocal (having the same foci) design, i.e. the detected X-rays are only emitted from the overlap of the two focal spots. This increases spatial resolution and reduce s background. The integration of the X-ray optics increases the signal-to-noise and thereby increases the sensitivity of the analysis for low-level analytes. This work will address a key need for radiochemical analysis of high-level waste using a non-destructive, multi-element, and rapid method in a radiation environment. There is significant potential that this instrumentation could be capable of on-line analysis for process waste stream characterization at DOE sites.

  3. Radiochemical Analysis by High Sensitivity Dual-Optic Micro X-ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, George J.; Gao, Ning

    2004-06-01

    A novel dual-optic micro X-ray fluorescence instrument will be developed to do radiochemical analysis of high-level radioactive wastes at DOE sites such as Savannah River Site and Hanford. This concept incorporates new X-ray optical elements such as monolithic polycapillaries, which focus X-rays. The polycapillary optic can be used to focus X-rays emitted by the X-ray tube thereby increasing the X-ray flux on the sample over 1000 times. The polycapillary optic will also be used to collect the X-rays from the excitation site. This will effectively screen the radiation background from the radioactive species in the specimen. This dual-optic approach significantly reduces the background and increases the analyte signal thereby increasing the sensitivity of the analysis. This dual-capillary design is essentially a confocal (having the same foci) design, i.e. the detected X-rays are only emitted from the overlap of the two focal spots. This increases spatial resolution and reduces background. The integration of the X-ray optics increases the signal-to-noise and thereby increases the sensitivity of the analysis for low-level analytes. This work will address a key need for radiochemical analysis of high-level waste using a non-destructive, multi-element, and rapid method in a radiation environment. There is significant potential that this instrumentation could be capable of on-line analysis for process waste stream characterization at DOE sites.

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

    Directory of Open Access Journals (Sweden)

    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.

  5. Characteristics of X-ray fluorescence of nuclear materials

    Energy Technology Data Exchange (ETDEWEB)

    Park, Seunghoon; Kwak, Sung-Woo; Shin, Jung-Ki; Park, Uk-Rayng; Jung, Heejun [Korea Institute of Nuclear Nonproliferation and Control, Daejeon (Korea, Republic of)

    2015-10-15

    LED is a technique of determination of uranium concentration as a continuous X-ray energy beams transmit a uranium liquid sample for safeguards. Compared to K-edge densitometer, due to relatively lower energy (L-edge energy is 17.17 keV) of Uranium L series energy than K-series energy, L-edge densitometer does not require high purity germanium detector with liquid nitride cooling. Therefore, the Ledge densitometer is appropriate for portable equipment for on-site nuclear material inspection and safeguards at facility sites. XRF combined with LED is a technique of finding of nuclear materials from reflected characteristic X-ray photons. In this study, characteristics of XRF of nuclear materials are simulated Monte Carlo method (Geant4) for feasibility of the system for determination of concentration of nuclear species. The analysis method of uranium concentration or minor actinides is applied using combination of linear extrapolation from jump of L-edge of sample and ratio between uranium and minor actinide from XRF measurement. In this study, The XRF ch aracteristics was simulated from Monte Carlo method. The peaks were obtained from nuclear material mixture. The estimated nuclear material concentration is low due to the volume effect of the sample. The correction factor or minimization of the effect is required.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  7. Quantitative analysis results of CE-1 X-ray fluorescence spectrometer ground base experiment

    Institute of Scientific and Technical Information of China (English)

    CUI Xing-Zhu; GAO Min; YANG Jia-Wei; WANG Huan-Yu; ZHANG Cheng-Mo; CHEN Yong; ZHANG Jia-Yu; PENG Wen-Xi; CAO Xue-Lei; LIANG Xiao-Hua; WANG Jin-Zhou

    2008-01-01

    As the nearest celestial body to the earth, the moon has become a hot spot again in astronomy field recently. The element analysis is a much important subject in many lunar projects. Remote X-ray spectrometry plays an important role in the geochemical exploration of the solar bodies. Because of th equasi-vacuum atmosphere on the moon, which has no absorption of X-ray, the X-ray fluorescence analysis is an effective way to determine the elemental abundance of lunar surface. The CE-1 X-ray fluorescence spectrometer (CE-1/XFS) aims to map the major elemental compositions on the lunar surface. This paper describes a method for quantitative analysis of elemental compositions. A series of ground base experiments are done to examine the capability of XFS. The obtained results, which show a reasonable agreement with the certified values at a 30% uncertainty level for major elements, are presented.

  8. Age Determination by X-ray Fluorescence Rubidium-Strontium Ratio Measurement in Lepidolite.

    Science.gov (United States)

    Herzog, L F

    1960-07-29

    X-ray fluorescence analysis of several lepidolites whose rubidium and strontium concentrations had already been determined by neutron activation and stable isotope dilution, or both, indicates that this technique can be used for rapid nondestructive reconnaissance rubidiumstrontium studies, and that an x-ray analysis method comparable in accuracy to isotope dilution can probably be developed for dating Precambrian lepidolites, as the simple technique presently used has many obvious possibilities for improvement.

  9. Project Title: Radiochemical Analysis by High Sensitivity Dual-Optic Micro X-ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, George J.; Gao, Ning

    2002-06-01

    A novel dual-optic micro X-ray fluorescence instrument will be developed to do radiochemical analysis of high-level radioactive wastes at DOE sites such as Savannah River Site and Hanford. This concept incorporates new X-ray optical elements such as monolithic polycapillaries and double bent crystals, which focus X-rays. The polycapillary optic can be used to focus X-rays emitted by the X-ray tube thereby increasing the X-ray flux on the sample over 1000 times. Polycapillaries will also be used to collect the X-rays from the excitation site and screen the radiation background from the radioactive species in the specimen. This dual-optic approach significantly reduces the background and increases the analyte signal thereby increasing the sensitivity of the analysis. A doubly bent crystal used as the focusing optic produces focused monochromatic X-ray excitation, which eliminates the bremsstrahlung background from the X-ray source. The coupling of the doubly bent crystal for monochromatic excitation with a polycapillary for signal collection can effectively eliminate the noise background and radiation background from the specimen. The integration of these X-ray optics increases the signal-to-noise and thereby increases the sensitivity of the analysis for low-level analytes. This work will address a key need for radiochemical analysis of high-level waste using a non-destructive, multi-element, and rapid method in a radiation environment. There is significant potential that this instrumentation could be capable of on-line analysis for process waste stream characterization at DOE sites.

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

    Science.gov (United States)

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

    2016-10-01

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

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

    Institute of Scientific and Technical Information of China (English)

    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.

  12. 3D micro-XRF for cultural heritage objects: new analysis strategies for the investigation of the Dead Sea Scrolls.

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Khuder, A. [Department of Chemistry, Atomic Energy Commission, P.O. Box 6091, Damascus (Syrian Arab Republic)], E-mail: scientific2@aec.org.sy; Sawan, M.Kh.; Karjou, J. [Department of Chemistry, Atomic Energy Commission, P.O. Box 6091, Damascus (Syrian Arab Republic); Razouk, A.K. [Department of Agriculture, Atomic Energy Commission, P.O. Box 6091, Damascus (Syrian Arab Republic)

    2009-07-15

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

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

    Science.gov (United States)

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

    2009-07-01

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

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

    Science.gov (United States)

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

    2004-01-07

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

  16. A new X-ray pinhole camera for energy dispersive X-ray fluorescence imaging with high-energy and high-spatial resolution

    Energy Technology Data Exchange (ETDEWEB)

    Romano, F.P., E-mail: romanop@lns.infn.it [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Altana, C. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Via S. Sofia 64, 95123 Catania (Italy); Cosentino, L.; Celona, L.; Gammino, S.; Mascali, D. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Pappalardo, L. [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Rizzo, F. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Via S. Sofia 64, 95123 Catania (Italy)

    2013-08-01

    A new X-ray pinhole camera for the Energy Dispersive X-ray Fluorescence (ED-XRF) imaging of materials with high-energy and high-spatial resolution, was designed and developed. It consists of a back-illuminated and deep depleted CCD detector (composed of 1024 × 1024 pixels with a lateral size of 13 μm) coupled to a 70 μm laser-drilled pinhole-collimator, positioned between the sample under analysis and the CCD. The X-ray pinhole camera works in a coaxial geometry allowing a wide range of magnification values. The characteristic X-ray fluorescence is induced on the samples by irradiation with an external X-ray tube working at a maximum power of 100 W (50 kV and 2 mA operating conditions). The spectroscopic capabilities of the X-ray pinhole camera were accurately investigated. Energy response and energy calibration of the CCD detector were determined by irradiating pure target-materials emitting characteristic X-rays in the energy working-domain of the system (between 3 keV and 30 keV). Measurements were performed by using a multi-frame acquisition in single-photon counting. The characteristic X-ray spectra were obtained by an automated processing of the acquired images. The energy resolution measured at the Fe–Kα line is 157 eV. The use of the X-ray pinhole camera for the 2D resolved elemental analysis was investigated by using reference-patterns of different materials and geometries. The possibility of the elemental mapping of samples up to an area of 3 × 3 cm{sup 2} was demonstrated. Finally, the spatial resolution of the pinhole camera was measured by analyzing the profile function of a sharp-edge. The spatial resolution determined at the magnification values of 3.2 × and 0.8 × (used as testing values) is about 90 μm and 190 μm respectively. - Highlights: • We developed an X-ray pinhole camera for the 2D X-ray fluorescence imaging. • X-ray spectra are obtained by a multi-frame acquisition in single photon mode. • The energy resolution in the X-ray

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-04-21

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-09-15

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

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

    Science.gov (United States)

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

    2017-03-01

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

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

    Indian Academy of Sciences (India)

    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.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

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

    Science.gov (United States)

    1989-06-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-08-08

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

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

    Science.gov (United States)

    Garmay, Andrey V.; Oskolok, Kirill V.

    2017-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Cordes, Nikolaus L., E-mail: ncordes@lanl.gov [Polymers and Coatings Group, Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Seshadri, Srivatsan, E-mail: srivatsan.seshadri@zeiss.com [Carl Zeiss X-ray Microscopy, Inc., Pleasanton, CA 94588 (United States); Havrilla, George J. [Chemical Diagnostics and Engineering, Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Yuan, Xiaoli [Julius Kruttschnitt Mineral Research Centre, University of Queensland, Indooroopilly, Brisbane, QLD 4068 (Australia); Feser, Michael [Carl Zeiss X-ray Microscopy, Inc., Pleasanton, CA 94588 (United States); Patterson, Brian M. [Polymers and Coatings Group, Material Science and Technology Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2015-01-01

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    Collins, Michael L [Los Alamos National Laboratory; Havrilla, George J [Los Alamos National Laboratory

    2009-01-01

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

  8. Fluorescence versus X-ray cholangiography during laparoscopic cholecystectomy

    DEFF Research Database (Denmark)

    Lehrskov, Lars Lang; Larsen, Søren S; Kristensen, Billy B;

    2016-01-01

    INTRODUCTION: Intraoperative fluorescent cholangiography is a novel non-invasive imaging technique to visualise the extrahepatic biliary tract during laparoscopic cholecystectomy. It has been proven feasible, fast and cost effective. Never-theless, there is only sparse data on the capacity......-ray cholangiography. This may lead to the introduction of online imaging of the extrahepatic tract during dissection of the gallbladder during cholecystectomy. FUNDING: none. TRIAL REGISTRATION: This study was registered with clinicaltrials.gov (No. NCT02344654), with the National Committee on Health Research Ethics...

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2017-02-07

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

  12. X-Ray Fluorescence Analysis for Barium, Zinc, Calcium and Phosphorus in Oil Additives.

    Science.gov (United States)

    1983-08-01

    HOAlD-I’ 908 XRAY FLUORESCENCE ANALYSIS FOR BARIUM ZINC CALCIUM AND i/i PHOSPHORUS IN OIL HDDITIVES(U MATERIALS RESEARCH LABS ASCOT VALE (AUSTRALIA...film technique was used by McGinness, Scott and Mortensen [101 for the quantitative x-ray emission analysis of paints . The paint films, "one-half mil

  13. Elemental analysis of various biomass solid fractions in biorefineries by X-ray fluorescence spectrometry

    DEFF Research Database (Denmark)

    Le, Duy Michael; Sorensen, Hanne R.; Meyer, Anne S.

    2017-01-01

    Elemental analysis by X-ray fluorescence spectrometry (XRF) of solid samples from a biorefinery process was performed to study the behaviour of mineral elements in a process involving hydrothermal pretreatment of biomass (wheat straw, corn stover, sugarcane bagasse, palm oil empty fruit bunches...

  14. Quantitative analysis by synchrotron radiation induced X-ray fluorescence at lure

    Science.gov (United States)

    Chevallier, P.; Brissaud, I.; Wang, J. X.

    1990-04-01

    The main features that makes synchrotron radiation an ideal source for X-ray fluorescence analysis are emphasized. Examples of quantitative analysis are given and a new type of spectrometer taking advantage of the focusing properties of a flat mosaic crystal and a position sensitive detector is described.

  15. X-ray fluorescence analysis study. Final report, December 1, 1970-December 31, 1977

    Energy Technology Data Exchange (ETDEWEB)

    Kneip, T J; Laurer, G R

    1978-01-01

    This report has described the most significant experiments and the results obtained, during the development of a system for the detection and measurement of Pb in blood using radioisotope-excited x-ray fluorescence analysis, over the contract period. Briefly, the report described: detector selection; source selection; source-sample-detector geometry; sample preparation; system calibration; and separation technique. (PSB)

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

    Energy Technology Data Exchange (ETDEWEB)

    Ning Gao

    2006-05-12

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

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

    Science.gov (United States)

    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.…

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

    Institute of Scientific and Technical Information of China (English)

    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.

  19. Modelling of the X-ray fluorescence from Mercury's surface and sodium exosphere

    Science.gov (United States)

    Cooper, Rose

    2016-10-01

    We model the fluorescent X-ray signal expected from the Mercury surface. Due to the high solar flux at Mercury, it represents a highly suitable target. Observations of this fluorescence will be performed by the Mercury Imaging X-ray Spectrometer (MIXS) on the upcoming BepiColumbo mission. Accurate modelling is required to plan observation strategies and eventually to quantify the surface composition. In addition, we also investigate the possibility of detecting fluorescence from the exosphere. We are using code modified from that used for the SMART-1 D-CIXS instrument to the Moon. Modifications include detector parameters, solar proximity, likely surface elemental components, and emission from the optically thin exosphere. Modelling of fluorescence from both the surface and exosphere are conducted, with particular emphasis on the sodium component.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  2. Trends in hard X-ray fluorescence mapping: environmental applications in the age of fast detectors

    Energy Technology Data Exchange (ETDEWEB)

    Lombi, E.; Donner, E. [University of South Australia, Centre for Environmental Risk Assessment and Remediation, Mawson Lakes, South Australia (Australia); CRC CARE, PO Box 486, Salisbury, South Australia (Australia); Jonge, M.D. de; Paterson, D. [Australian Synchrotron, X-ray Fluorescence Microscopy, 800 Blackburn Road, Clayton, Victoria (Australia); Ryan, C.G. [CSIRO Earth Science and Resource Engineering, Normanby Road, Clayton, Victoria (Australia)

    2011-06-15

    Environmental samples are extremely diverse but share a tendency for heterogeneity and complexity. This heterogeneity poses methodological challenges when investigating biogeochemical processes. In recent years, the development of analytical tools capable of probing element distribution and speciation at the microscale have allowed this challenge to be addressed. Of these available tools, laterally resolved synchrotron techniques such as X-ray fluorescence mapping are key methods for the in situ investigation of micronutrients and inorganic contaminants in environmental samples. This article demonstrates how recent advances in X-ray fluorescence detector technology are bringing new possibilities to environmental research. Fast detectors are helping to circumvent major issues such as X-ray beam damage of hydrated samples, as dwell times during scanning are reduced. They are also helping to reduce temporal beamtime requirements, making particularly time-consuming techniques such as micro X-ray fluorescence ({mu}XRF) tomography increasingly feasible. This article focuses on {mu}XRF mapping of nutrients and metalloids in environmental samples, and suggests that the current divide between mapping and speciation techniques will be increasingly blurred by the development of combined approaches. (orig.)

  3. Trends in hard X-ray fluorescence mapping: environmental applications in the age of fast detectors.

    Science.gov (United States)

    Lombi, E; de Jonge, M D; Donner, E; Ryan, C G; Paterson, D

    2011-06-01

    Environmental samples are extremely diverse but share a tendency for heterogeneity and complexity. This heterogeneity poses methodological challenges when investigating biogeochemical processes. In recent years, the development of analytical tools capable of probing element distribution and speciation at the microscale have allowed this challenge to be addressed. Of these available tools, laterally resolved synchrotron techniques such as X-ray fluorescence mapping are key methods for the in situ investigation of micronutrients and inorganic contaminants in environmental samples. This article demonstrates how recent advances in X-ray fluorescence detector technology are bringing new possibilities to environmental research. Fast detectors are helping to circumvent major issues such as X-ray beam damage of hydrated samples, as dwell times during scanning are reduced. They are also helping to reduce temporal beamtime requirements, making particularly time-consuming techniques such as micro X-ray fluorescence (μXRF) tomography increasingly feasible. This article focuses on μXRF mapping of nutrients and metalloids in environmental samples, and suggests that the current divide between mapping and speciation techniques will be increasingly blurred by the development of combined approaches.

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

    CERN Document Server

    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%.

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

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

    2016-10-08

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2016-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2015-05-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Taborda, A.; Desbrée, A. [Institut de Radioprotection et de Sûreté Nucléaire (IRSN), PRP-HOM/SDI/LEDI, BP-17, 31, Avenue de la Division Leclerc, 92262 Fontenay-aux-Roses (France); Carvalho, A. [IEQUALTECS, Lda, Rua Dr. Francisco Sá Carneiro, 36, 2500-065 S. Gregório CLD (Portugal); Chaves, P.C. [C" 2TN, Campus Tecnológico e Nuclear, Instituto Superior Técnico, Universidade de Lisboa, EN10 km 139.7, 2685-066 Bobadela LRS (Portugal); Reis, M.A., E-mail: mareis@ctn.tecnico.ulisboa.pt [IEQUALTECS, Lda, Rua Dr. Francisco Sá Carneiro, 36, 2500-065 S. Gregório CLD (Portugal); C" 2TN, Campus Tecnológico e Nuclear, Instituto Superior Técnico, Universidade de Lisboa, EN10 km 139.7, 2685-066 Bobadela LRS (Portugal)

    2016-08-15

    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 10{sup 3} 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 {sup 57}Co, 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.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Cheong, Seong-Kyun; Jones, Bernard L; K Siddiqi, Arsalan; Liu, Fang; Manohar, Nivedh; Cho, Sang Hyun [Nuclear and Radiological Engineering and Medical Physics Programs, Woodruff School of Mechanical Engineering, Georgia Institute of Technology, Atlanta, GA 30332 (United States)], E-mail: scho@gatech.edu

    2010-02-07

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

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

    Science.gov (United States)

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

    2010-02-07

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2015-11-01

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

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

    Science.gov (United States)

    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.

  19. Application of X-Ray Fluorescence Analysis in Investigations of Historical Monuments

    Directory of Open Access Journals (Sweden)

    T. Čechák

    2005-01-01

    Full Text Available Nuclear techniques and other techniques using ionising radiation represent a valuable tool in non-destructive diagnostics applied to archaeological finds and objects of arts, namely for determining the composition of materials used in the production of artefacts. X-ray fluorescence analysis, both in its energy form and in its wave dispersive form, is one of the most widespread methods using ionising radiation to study the elemental composition of materials. It is frequently used for studies of various cultural and historic relicts and objects of art. This work summarizes the authors’ experience with X-ray fluorescence analysis in investigating historical frescos namely by means of portable provide spectroscopic devices. The results of these measurements information on the composition of the pigments, enable the comparison of processes used in the fabrication of pigments by individual artists, and in many cases offer information on how to repair the damaged parts. 

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, T. [National University of Mexico, Faculty of Chemistry, Building D, CU (O4510) Mexico, D.F. Mexico (Mexico)], E-mail: tmc@servidor.unam.mx; Lartigue, J. [National University of Mexico, Faculty of Chemistry, Building D, CU (O4510) Mexico, D.F. Mexico (Mexico); Zarazua, G.; Avila-Perez, P. [National Institute of Nuclear Research. Carr. Mexico-Toluca Km 36.5, (52045) Salazar, Ocoyoacac, Edo. de Mexico (Mexico); Navarrete, M. [National University of Mexico, Faculty of Chemistry, Building D, CU (O4510) Mexico, D.F. Mexico (Mexico); Tejeda, S. [National Institute of Nuclear Research. Carr. Mexico-Toluca Km 36.5, (52045) Salazar, Ocoyoacac, Edo. de Mexico (Mexico)

    2008-12-15

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

  2. Determination of catalyst metal residues in polymers by X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Bichinho, Katia M. [CIENTEC-Fundacao de Ciencia e Tecnologia, Rua Washington Luiz, 675, Porto Alegre, 90010-460 (Brazil); Pires, Gilvan Pozzobon [Instituto de Quimica, Universidade Federal do Rio Grande do Sul (UFRGS) Avenida Bento Goncalves 9500, Porto Alegre, 91501-970 (Brazil); Stedile, Fernanda C. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul (UFRGS) Avenida Bento Goncalves 9500, Porto Alegre, 91501-970 (Brazil); Santos, Joao Henrique Z. dos [Instituto de Quimica, Universidade Federal do Rio Grande do Sul (UFRGS) Avenida Bento Goncalves 9500, Porto Alegre, 91501-970 (Brazil)]. E-mail: jhzds@iq.ufrgs.br; Wolf, Carlos Rodolfo [Ipiranga Petroquimica S.A., Departamento de Desenvolvimento de Produto, Polo Petroquimico do Sul, BR 386, km 419, Triunfo, CEP 95853-000 (Brazil)

    2005-06-30

    Commercial polyethylenes produced by Ziegler-Natta, Philips and metallocene technology were analyzed by X-ray fluorescence spectroscopy. Synthetic standards using wax matrix was shown to be suitable for the calibration curve in comparison to those prepared by milling and grinding virgin polymer mixed with standard metal oxide as matrix. The detection limits obtained for the studied metal in the different polymers were: 12 mg kg{sup -1} for Mg, 0.8 mg kg{sup -1} for Ti, 1.6 mg kg{sup -1} for Cr, 1.2 mg kg{sup -1} for Zr and 1.9 mg kg{sup -1} for V. For comparative reasons, the determination of residual metal content by Rutherford backscattering spectrometry (RBS) and total-reflection X-ray fluorescence spectrometry (TXRF) is also discussed.

  3. Macro and micro full field x-ray fluorescence with an X-ray pinhole camera presenting high energy and high spatial resolution.

    Science.gov (United States)

    Romano, Francesco Paolo; Caliri, Claudia; Cosentino, Luigi; Gammino, Santo; Giuntini, Lorenzo; Mascali, David; Neri, Lorenzo; Pappalardo, Lighea; Rizzo, Francesca; Taccetti, Francesco

    2014-11-01

    This work describes a tabletop (50 cm × 25 cm × 25 cm) full field X-ray pinhole camera (FF-XPC) presenting high energy- and high spatial-resolution. The FF-XPC consists of a conventional charge-coupled device (CCD) detector coupled, in a coaxial geometry, to a pinhole collimator of small diameter. The X-ray fluorescence (XRF) is induced on the samples with an external low-power X-ray tube. The use of the CCD as an energy dispersive X-ray detector was obtained by adopting a multi-image acquisition in single photon counting and by developing a processing algorithm to be applied in real-time to each of the acquired image-frames. This approach allowed the measurement of X-ray spectra with an energy resolution down to 133 eV at the reference value of 5.9 keV. The detection of the X-ray fluorescence through the pinhole-collimator allowed the two-dimensional elemental mapping of the irradiated samples. Two magnifications (M), determined by the relative sample-pinhole-CCD distances, are used in the present setup. A low value of M (equal to 0.35×) allows the macro-FF-XRF of large area samples (up to 4 × 4 cm(2)) with a spatial resolution down to 140 μm; a large magnification (M equal to 6×) is used for the micro-FF-XRF of small area samples (2.5 × 2.5 mm(2)) with a spatial resolution down to 30 μm.

  4. In-lab X-ray fluorescence and diffraction techniques for pathological calcifications

    OpenAIRE

    Rouzière, Stéphan; Bazin, Dominique; Daudon, Michel

    2016-01-01

    International audience; If imaging by physical methods is probably the best well-known link between physics and medicine, other ways such as X-ray fluorescence and diffraction techniques give significant information to clinicians. In this contribution, we would like to assess different results obtained through such techniques on three main problems in urology namely Randall's plaque, brushite kidney stones and phase conversion between weddellite and whewellite. Randall's plaque is a mineral d...

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  6. Determination of Fission Products in Irradiated Fuel by X-Ray Fluorescence

    DEFF Research Database (Denmark)

    Mogensen, Mogens Bjerg; Als-Nielsen, Jens Aage; Andersen, Niels Hessel

    X-ray fluorescence i s a well e s t a b l i s h e d analytical tool for measuring elemental composition of fairly large (~ 5 cm2) "cold" samples. A version of t h i s technique has been developed for a n a l y s i s of radial d i s t r i b u t i o n of f i s s i o n products Xe, Cs and Ba in irra...

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

    Science.gov (United States)

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

    2007-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Wu Di; Li Yuhua; Wong, Molly D.; Liu Hong [Center for Bioengineering and School of Electrical and Computer Engineering, University of Oklahoma, Norman, Oklahoma 73019 (United States)

    2013-05-15

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

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

    CERN Document Server

    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...

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

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

  13. Semi-empirical model for fluorescence lines evaluation in diagnostic x-ray beams.

    Science.gov (United States)

    Bontempi, Marco; Andreani, Lucia; Labanti, Claudio; Costa, Paulo Roberto; Rossi, Pier Luca; Baldazzi, Giuseppe

    2016-01-01

    Diagnostic x-ray beams are composed of bremsstrahlung and discrete fluorescence lines. The aim of this study is the development of an efficient model for the evaluation of the fluorescence lines. The most important electron ionization models are analyzed and implemented. The model results were compared with experimental data and with other independent spectra presented in the literature. The implemented peak models allow the discrimination between direct and indirect radiation emitted from tungsten anodes. The comparison with the independent literature spectra indicated a good agreement.

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

    Science.gov (United States)

    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.

  15. Monochromatic wavelength dispersive x-ray fluorescence providing sensitive and selective detection of uranium

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, George J [Los Alamos National Laboratory; Collins, Michael L [Los Alamos National Laboratory; Montoya, Velma M [Los Alamos National Laboratory; Chen, Zewu [XOS; Wei, Fuzhong [XOS

    2010-01-01

    Monochromatic wavelength dispersive X-ray fluorescence (MWDXRF) is a sensitive and selective method for elemental compositional analyses. The basis for this instrumental advance is the doubly curved crystal (DCC) optic. Previous work has demonstrated the feasibility of sensitive trace element detection for yttrium as a surrogate for curium in aqueous solutions. Additional measurements have demonstrated similar sensitivity in several different matrix environments which attests to the selectivity of the DCC optic as well as the capabilities of the MWDXRF concept. The objective of this effort is to develop an improved Pu characterization method for nuclear fuel reprocessing plants. The MWDXRF prototype instrument is the second step in a multi-year effort to achieve an improved Pu assay. This work will describe a prototype MWDXRF instrument designed for uranium detection and characterization. The prototype consists of an X-ray tube with a rhodium anode and a DCC excitation optic incorporated into the source. The DCC optic passes the RhK{alpha} line at 20.214 keV for monochromatic excitation of the sample. The source is capable of 50 W power at 50 kV and 1.0 mA operation. The x-ray emission from the sample is collected by a DCC optic set at the UL{alpha} line of 13.613 keV. The collection optic transmits the UL{alpha} x-rays to the silicon drift detector. The x-ray source, sample, collection optic and detector are all mounted on motion controlled stages for the critical alignment of these components. The sensitivity and selectivity of the instrument is obtained through the monochromatic excitation and the monochromatic detection. The prototype instrument performance has a demonstrated for sensitivity for uranium detection of around 2 ppm at the current state of development. Further improvement in sensitivity is expected with more detailed alignment.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    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)

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

    Science.gov (United States)

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

    2017-01-01

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

  1. Scanning protein analysis of electrofocusing gels using X-ray fluorescence.

    Science.gov (United States)

    Matsuyama, Satoshi; Matsunaga, Akihiro; Sakamoto, Shinichi; Iida, Yutaka; Suzuki, Yoshinari; Ishizaka, Yukihito; Yamauchi, Kazuto; Ishikawa, Tetsuya; Shimura, Mari

    2013-05-01

    Recently, "metallomics," in addition to genomics and proteomics, has become a focus as a novel approach to identify sensitive fluctuations in homeostasis that accompany metabolic processes, such as stress responses, differentiation, and proliferation. Cellular elements and associated protein behavior provide important clues for understanding cellular and disease mechanism(s). It is important to develop a system for measuring the native status of the protein. In this study, we developed an original freeze-dried electrofocusing native gel over polyimide film (native-gel film) for scanning protein analysis using synchrotron radiation excited X-ray fluorescence (SPAX). To our knowledge, this is the first report detailing the successful mapping of metal-associated proteins of electrofocusing gels using X-ray fluorescence. SPAX can provide detection sensitivity equivalent to that of LA-ICP-MS. In addition to this increased sensitivity, SPAX has the potential to be combined with other X-ray spectroscopies. Our system is useful for further applications in proteomics investigating cellular element-associated protein behaviors and disease mechanisms.

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

    Energy Technology Data Exchange (ETDEWEB)

    Naghedolfeizi, M.; Chung, J.S.; Ice, G.E. [Oak Ridge National Lab., TN (United States). Metals and Ceramics Div.; Yun, W.B.; Cai, Z.; Lai, B. [Argonne National Lab., IL (United States). Advanced Photon Source

    1998-12-31

    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 {approximately} 1 x 3 {micro}m{sup 2} 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 {micro}m 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.

  3. Capillary electrophoresis micro X-ray fluorescence: a tool for benchtop elemental analysis.

    Science.gov (United States)

    Miller, Thomasin C; Joseph, Martha R; Havrilla, George J; Lewis, Cris; Majidi, Vahid

    2003-05-01

    A new tool was developed for separation and elemental detection by interfacing a simple capillary electrophoresis (CE) apparatus, constructed using a thin-walled fused-silica capillary, with a benchtop energy-dispersive micro X-ray fluorescence (MXRF) system. X-ray excitation and detection of the separated analytes was done using an EDAX Eagle II micro X-ray fluorescence system equipped with a polycapillary Rh target excitation source and a SiLi detector. It was demonstrated that this prototype system could be used for the separation and detection of species containing two different metals from one another, specifically Cu and Co. Free Co could also be separated from Co bound to cyanocobalamin (vitamin B-12). Two organic compounds were also separated from one another, a large biological protein, ferritin, from a small biological organic, cyanocobalamin. Preliminary average detection limits obtained on this system were on the order of 10(-)(4) M and compared favorably to those reported for the similar technique of CE-synchrotron XRF. CEMXRF allows for nondestructive, simultaneous, on-line, benchtop elemental analysis for chemical speciation applications.

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

    Energy Technology Data Exchange (ETDEWEB)

    Hoover, Andrew S [Los Alamos National Laboratory; Rudy, Cliff R [Los Alamos National Laboratory; Tobin, Steve J [Los Alamos National Laboratory; Charlton, William S [Los Alamos National Laboratory; Stafford, A [TEXAS A& M; Strohmeyer, D [TEXAS A& M; Saavadra, S [ORNL

    2009-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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. Metals determination in wood treated by synchrotron radiation X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Vives, Ana Elisa Sirito de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Silva, Richard Maximiliano da Cunha [Centro de Energia Nuclear na Agricultura, Piracicaba, SP (Brazil)]. E-mail: maxcunha@cena.usp.br; Medeiros, Jean Gabriel da Silva; Tomazello Filho, Mario [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz]. E-mail: jeangm@esalq.usp.br; mtomazel@esalq.usp.br; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo]. E-mail: Silvana@fec.unicamp.br; Zucchi, Orgheda Luiza Araujo Domingues [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Barroso, Regina Cely [Universidade do Estado, Rio de Janeiro, RJ (Brazil)]. E-mail: cely@uerj.br

    2005-07-01

    The paper describes the use of X-Ray fluorescence analysis for distribution and quantification of metals in the hardwood (Eucalyptus sp) and softwood (Pinus sp) treated with CCA (copper-chromium-arsenic). The sapwood/heartwood for hardwood sample and the growth-rings for softwood sample were analyzed. The samples were scanned in 320 mm steps in the vertical direction. For excitation of the elements a white beam synchrotron radiation of {approx} 320 x 180 mm was employed and for the X-ray detection a Si(Li) semiconductor detector. The elements K, Ca, Cr, Mn, Cu, Zn and As were determined. Fundamental parameters were used to quantify the elements concentrations. (author)

  7. Elemental distribution images in prostate samples by X-ray fluorescence microtomography

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, G.R. [Non-destructive Testing, Corrosion and Welding Laboratory, PEMM/COPPE/UFRJ, Rio de Janeiro (Brazil); Rocha, H.S. [Nuclear Instrumentation Laboratory, PEN/COPPE/UFRJ, P.O. Box 68509, 21.941-972, Rio de Janeiro (Brazil); Anjos, M.J. [Physics Institute-Stated University of Rio de Janeiro, Rio de Janeiro (Brazil); Lima, I. [Nuclear Instrumentation Laboratory, PEN/COPPE/UFRJ, P.O. Box 68509, 21.941-972, Rio de Janeiro (Brazil); Lopes, R.T., E-mail: ricardo@lin.ufrj.br [Nuclear Instrumentation Laboratory, PEN/COPPE/UFRJ, P.O. Box 68509, 21.941-972, Rio de Janeiro (Brazil)

    2012-07-15

    An X-ray transmission microtomography (CT) system combined with an X-ray fluorescence microtomography (XRF{mu}CT) system was implemented in the Brazilian Synchrotron Light Laboratory (LNLS), in order to determine the elemental distribution in prostate samples aiming at establishing a correlation between the concentration of some elements and the characteristics and pathology of the tissues. The CT images were reconstructed using a filtered-back projection algorithm and the XRF{mu}CT images were reconstructed using a filtered-back projection algorithm with absorption corrections. - Highlights: Black-Right-Pointing-Pointer In this study we evaluated prostate tissues by microtomography imaging techniques. Black-Right-Pointing-Pointer The elemental distribution of iron, copper and zinc was obtained in each sample. Black-Right-Pointing-Pointer The great advantage of this technique is the visualization in three-dimension. Black-Right-Pointing-Pointer The elemental distribution visualization was obtained without damaging the material.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, M.S.; Domingues, M.D.L.F.; Mantovano, J.L.; Filho, E.Q.S. [Instituto de Engenharia Nuclear, CNEN-RJ, CP 68550, 21945-590 (Brazil)

    1998-12-28

    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 {mu}g/l of uranium the coefficient of variation for five measurements is 5% and the detection limit is 5.5 {mu}g/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.)

  11. Trace element determination in amniotic fluid by total reflection X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Greaves, E.D.; Sajo-Bohus, L.; Castelli, C.; Borgerg, C. [Universidad Simon Bolivar, Caracas (Venezuela); Meitin, J.; Liendo, J.

    1995-03-01

    A new method is reported for the determination of Fe, Cu, Zn, and Br in amniotic fluid (AF) by Total Reflection X-Ray Fluorescence. The irradiation of AF samples with monochromatic X-Rays reduces the scattering background from the organic matrix and avoids the need for sample digestion. Sample manipulation is reduced to centrifuging and adding cobalt as internal standard. Lower detection limits obtained are 109, 53, 44 and 37 ppb for Fe, Cu, Zn and Br respectively. Measurement precision depends on element concentrations and can be as low as 1.5% SD. Results of the analysis of 34 AF samples from Venezuelan pregnant patients agree with previously reported ranges of Fe, Cu and Zn. Other elements observed but not quantified are Cl, K, Ca in all spectra and Pb and Sr in some of them. (author).

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

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Andre Pereira de; Braz, Delson; Mota, Carla Lemos, E-mail: apalmeid@gmail.co, E-mail: delson@lin.ufrj.b, E-mail: clemos@con.ufrj.b [Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Nuclear; Oliveira, Luis Fernando de; Barroso, Regina Cely; Pinto, Nivia Graciele Villela, E-mail: cely@uerj.b, E-mail: lfolive@uerj.b, E-mail: nitatag@gmail.co [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Inst. de Fisica; Cardoso, Simone Coutinho, E-mail: simone@if.ufrj.b [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Inst. de Fisica; Moreira, Silvana, E-mail: silvana@fec.unicamp.b [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo

    2009-07-01

    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)

  13. Development of a reconstruction software of elemental maps by micro X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Andre Pereira de; Braz, Delson; Mota, Carla Lemos, E-mail: apalmeid@gmail.co, E-mail: delson@lin.ufrj.b, E-mail: clemos@con.ufrj.b [Universidade Federal do Rio de Janeiro (PEN/COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Programa de Energia Nuclear; Oliveira, Luis Fernando de; Barroso, Regina Cely; Pinto, Nivia Graciele Villela, E-mail: cely@uerj.b, E-mail: lfolive@uerj.b, E-mail: nitatag@gmail.co [Universidade do Estado do Rio de Janeiro (IF/UERJ), RJ (Brazil). Inst. de Fisica; Cardoso, Simone Coutinho [Universidade Federal do Rio de Janeiro (IF/UFRJ), RJ (Brazil). Inst. de Fisica; Moreira, Silvana [Universidade Estadual de Campinas (FEC/UNICAMP), SP (Brazil) Faculdade de Engenharia Civil, Arquitetura e Urbanismo

    2009-07-01

    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 at National Synchrotron Light Laboratory (LNLS), Brazil. Automatic 2D scans were performed and element distribution maps were obtained in form of a matrix of data. (author)

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

    Science.gov (United States)

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

    2009-11-15

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

  15. X-ray fluorescent lines from the Compton-thick AGN in M5

    CERN Document Server

    Xu, Weiwei; Gou, Lijun; Liu, Jiren

    2015-01-01

    The cold disk/torus gas surrounding AGN emits fluorescent lines when irradiated by hard X-ray photons. The fluorescent lines of elements other than Fe and Ni are rarely detected due to their relative faintness. We report the detection of K$\\alpha$ lines of neutral Si, S, Ar, Ca, Cr, and Mn, along with the prominent Fe K$\\alpha$, Fe K$\\beta$, and Ni K$\\alpha$ lines, from the deep Chandra observation of the low-luminosity Compton-thick AGN in M51. The Si K$\\alpha$ line at 1.74 keV is detected at $\\sim3\\sigma$, the other fluorescent lines have a significance between 2 and 2.5 $\\sigma$, while the Cr line has a significance of $\\sim1.5\\sigma$. These faint fluorescent lines are made observable due to the heavy obscuration of the intrinsic spectrum of M51, which is revealed by Nustar observation above 10 keV. The hard X-ray continuum of M51 from Chandra and Nustar can be fitted with a power-law spectrum with an index of 1.8, reprocessed by a torus with an equatorial column density of $N_{\\rm H}\\sim7\\times10^{24}$ cm...

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

    Science.gov (United States)

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

    2016-12-01

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

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

    Science.gov (United States)

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

    2016-12-21

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

  18. Application of synchrotron x-ray fluorescence microscopy to the study of multi-metal oxide ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Perry, D.L. [Lawrence Berkeley National Lab., CA (United States)]|[Univ. of California, Berkeley, CA (United States). G.T. Seaborg Inst. for Transactinium Science; McHugo, S.; Thompson, A.C. [Lawrence Berkeley National Lab., CA (United States)] [and others

    1998-12-31

    Synchrotron x-ray fluorescence microscopy has been used to study multi-metal oxide ceramics that have been designed to sequester radioactive actinide elements for long-term storage and disposal. X-ray fluorescent lines for the various elements have been used for lateral elemental mapping of the materials, and the heterogeneity of the samples is discussed with respect to the elements in the crystallographic phases that have previously been documented by other means of structural and chemical analyses.

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

    Energy Technology Data Exchange (ETDEWEB)

    Worley, Christopher G [Los Alamos National Laboratory

    2009-01-01

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

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

    Science.gov (United States)

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

    2009-04-21

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

  1. Synchrotron radiation micro-X-ray fluorescence analysis: A tool to increase accuracy in microscopic analysis

    CERN Document Server

    Adams, F

    2003-01-01

    Microscopic X-ray fluorescence (XRF) analysis has potential for development as a certification method and as a calibration tool for other microanalytical techniques. The interaction of X-rays with matter is well understood and modelling studies show excellent agreement between experimental data and calculations using Monte Carlo simulation. The method can be used for a direct iterative calculation of concentrations using available high accuracy physical constants. Average accuracy is in the range of 3-5% for micron sized objects at concentration levels of less than 1 ppm with focused radiation from SR sources. The end-station ID18F of the ESRF is dedicated to accurate quantitative micro-XRF analysis including fast 2D scanning with collection of full X-ray spectra. Important aspects of the beamline are the precise monitoring of the intensity of the polarized, variable energy beam and the high reproducibility of the set-up measurement geometry, instrumental parameters and long-term stability.

  2. Multilayers quantitative X-ray fluorescence analysis applied to easel paintings.

    Science.gov (United States)

    de Viguerie, Laurence; Sole, V Armando; Walter, Philippe

    2009-12-01

    X-ray fluorescence spectrometry (XRF) allows a rapid and simple determination of the elemental composition of a material. As a non-destructive tool, it has been extensively used for analysis in art and archaeology since the early 1970s. Whereas it is commonly used for qualitative analysis, recent efforts have been made to develop quantitative treatment even with portable systems. However, the interpretation of the results obtained with this technique can turn out to be problematic in the case of layered structures such as easel paintings. The use of differential X-ray attenuation enables modelling of the various layers: indeed, the absorption of X-rays through different layers will result in modification of intensity ratio between the different characteristic lines. This work focuses on the possibility to use XRF with the fundamental parameters method to reconstruct the composition and thickness of the layers. This method was tested on several multilayers standards and gives a maximum error of 15% for thicknesses and errors of 10% for concentrations. On a painting test sample that was rather inhomogeneous, the XRF analysis provides an average value. This method was applied in situ to estimate the thickness of the layers a painting from Marco d'Oggiono, pupil of Leonardo da Vinci.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-03-13

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Tiwari, M. K.; Singh, A. K.; Das, Gangadhar; Chowdhury, Anupam; Lodha, G. S.

    2014-04-01

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

  7. Determination of metals in lubricating oils by X-ray fluorescence spectrometry.

    Science.gov (United States)

    Pouzar, M; Cernohorský, T; Krejcová, A

    2001-06-21

    The determination of common wear metals, namely iron, chromium, copper, zinc and lead, in a wide range of lubricating oil samples was investigated for the use of a low-cost, wavelength-dispersive X-ray fluorescence spectrometer. The procedure provided results in satisfactory agreement with inductively coupled plasma spectrometry used as reference method after microwave digestion of the samples in concentrated nitric acid. Statistical tests following extensive regression analyses of the data indicated that interelement effects were not statistically significant and that a simple linear regression was adequate for the calibration of individual metals.

  8. A Fundamental Parameter-Based Calibration Model for an Intrinsic Germanium X-Ray Fluorescence Spectrometer

    DEFF Research Database (Denmark)

    Christensen, Leif Højslet; Pind, Niels

    1982-01-01

    secondary target a number of relative calibration constants are calculated on the basis of knowledge of the irradiation geometry, the detector specifications, and tabulated fundamental physical parameters. The absolute calibration of the spectrometer is performed by measuring one pure element standard per......A matrix-independent fundamental parameter-based calibration model for an energy-dispersive X-ray fluorescence spectrometer has been developed. This model, which is part of a fundamental parameter approach quantification method, accounts for both the excitation and detection probability. For each...

  9. Application of direct peak analysis to energy dispersive x-ray fluorescence spectra

    Energy Technology Data Exchange (ETDEWEB)

    Nielson, K.K.

    1977-07-01

    A modified Covell method for direct peak analysis has been applied to energy dispersive x-ray fluorescence spectra. The method is background independent and is well-suited to computerized data reduction. It provides acceptable precision, minimizes errors from instrumental gain shift, and permits peak overlap correction. Peak overlap errors exhibit both positive and negative nodes as a function of peak separation distance, and are corrected using concentration ratios determined from thin, single-element standards. Peak precisions and overlaps are evaluated as a function of window width to aid in width selection. Least-square polynomial smoothing prior to peak analysis significantly improves peak area precisions without significantly affecting their accuracies.

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

    Science.gov (United States)

    Borgese, Laura; Bilo, Fabjola; Tsuji, Kouichi; Fernández-Ruiz, Ramón; Margui, Eva; Streli, Christina; Pepponi, Giancarlo; Stosnach, Hagen; Yamada, Takashi; Vandenabeele, Peter; Maina, David M.; Gatari, Michael; Shepherd, Keith D.; Towett, Erick K.; Bennun, Leonardo; Custo, Graciela; Vasquez, Cristina; Depero, Laura E.

    2014-11-01

    Total Reflection X-Ray Fluorescence (TXRF) is a mature technique to evaluate quantitatively the elemental composition of liquid samples deposited on clean and well polished reflectors. In this paper the results of the first worldwide TXRF round-robin test of water samples, involving 18 laboratories in 10 countries are presented and discussed. The test was performed within the framework of the VAMAS project, interlaboratory comparison of TXRF spectroscopy for environmental analysis, whose aim is to develop guidelines and a standard methodology for biological and environmental analysis by means of the TXRF analytical technique.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  12. Twin image removal in X-ray fluorescence holography with two energies

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    In the last decade,X-ray fluorescence holography has been developed for the study of 3D atomic arrangements in solids.However,it encounters the twin image problem which may disturb the reconstructed atomic images.In this paper,the formation of twin image is discussed and we propose a modified two-energy algorithm to remove the twin image.The simulation shows that the method is valid and more efficient than the multiple-energy algorithm proposed by Barton.

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  15. X-ray fluorescence spectrometry determination of open-hearth furnace slag by pressed powder briquetting

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    A rapid analysis method of determining content of eight compounds of open-hearth furnace slag was developed using X-ray fluorescence spectrometry and pressed powder briquettes. Matrix effect was corrected using theoretical alpha coefficient. Grains-size effect was eliminated by optimized sample preparation technique parameters. Mineral effect was corrected with standard curve of specially made standard samples. The analysis results of TiO2, TFe, SiO2, MgO, Al2O3,CaO, MnO and P2O5 in slag samples showed that both precision and accuracy are comparable with that of chemical method.

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

    Science.gov (United States)

    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. Electrophoretic separation and detection of metalloproteins by X-ray fluorescence mapping.

    Science.gov (United States)

    Khare, Tripti; Chishti, Yasmin; Finney, Lydia A

    2012-01-01

    All living systems depend on metalloproteins. Yet, while tools for the separation and identification of apo-proteins are well developed, those enabling identification and quantitation of individual metalloproteins within complex mixtures are still nascent. Here, we describe the electrophoretic separation of a mixture of carbonic anhydrase, ceruloplasmin, urease, and hemoglobin using native 2D gel electrophoresis and X-ray fluorescence mapping-an approach we have developed to be broadly applicable, not require specialized equipment for sample preparation, and likely to be extensible in the future.

  18. Picoliter solution deposition for total reflection X-ray fluorescence analysis of semiconductor samples

    Energy Technology Data Exchange (ETDEWEB)

    Sparks, Chris M., E-mail: chris.sparks@svtc.co [Analytical Services, SVTC Technologies, Austin, TX 78741 (United States); Fittschen, Ursula E.A. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Institute of Inorganic and Applied Chemistry, University of Hamburg, 20146 Hamburg (Germany); Havrilla, George J. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2010-09-15

    A deposition system capable of delivering picoliter quantities of solution in programmable arrays was investigated as a method for sample preparation for total reflection X-ray fluorescence (TXRF) spectroscopy. Arrays of trace metals in solution were deposited on Si wafers. The array deposits provide a capability of depositing closely spaced (100 {mu}m or less), typically 5-20 {mu}m diameter droplets in an area that can be matched to the analysis spot of the TXRF detector. The dried depositions were physically characterized and the effect of deposition type and matrix on the TXRF signal was investigated.

  19. Waste reduction and process improvements in the analysis of plutonium by x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Worley, Christopher G [Los Alamos National Laboratory; Sodweberg, Constance B [Los Alamos National Laboratory; Townsend, Lisa E [Los Alamos National Laboratory

    2009-01-01

    Significant modifications were made to a sample preparation process for quantifying gallium in plutonium metal by wavelength dispersive X-ray fluorescence. These changes were made to minimize waste and improve process safety and efficiency. Sample sizes were reduced, cheaper sample preparation acids were used, and safety improvements were implemented. Using this modified process, results from analyzing a batch oftest samples indicated that relative precision and accuracy were {approx}0.2% and {approx}0.1% respectively, which is comparable to that obtained using the older, established sample preparation method.

  20. Use of X-ray Fluorescence Analysis for the Determination of Rare Earth Elements

    Science.gov (United States)

    Schramm, Rainer

    2016-09-01

    X-ray fluorescence spectrometry (XRF) is a powerful tool for the analysis of solid material. That is the reason why the technique was applied for the determination of rare earth elements (REEs) since about 1970. At present, energy-dispersive XRF and wavelength-dispersive XRF are used for the analysis of pressed powder pellets or fused Li-borate beads containing REEs. The production of reliable results can only be achieved by careful optimization of the parameter, in particular the selection of spectral lines. The quantification is based on a calibration realized by using reference samples.

  1. Mapping element distributions in plant tissues using synchrotron X-ray fluorescence techniques.

    Science.gov (United States)

    Donner, Erica; de Jonge, Martin D; Kopittke, Peter M; Lombi, Enzo

    2013-01-01

    Synchrotron-based X-ray fluorescence (XRF) is allowing substantial advances in several disciplines of plant science by allowing the in situ examination of elements within plant tissues. Continual improvements in detector speed, sensitivity, and resolution are increasing the diversity of questions that can be addressed using this technique, including the in situ analysis of elements (such as nutrients or toxicants) within fresh and hydrated tissues. Here, we describe the general principles for designing and conducting experiments for the examination of elemental distributions in plant material using micro-XRF.

  2. Portable X-ray fluorescence spectrometer system using a low-level radioisotope {sup 55}Fe

    Energy Technology Data Exchange (ETDEWEB)

    Shimoyama, Susumu [Kibi International Univ., Takahashi, Okayama (Japan); Noda, Yasuko [Den Material Co., Ltd., Color Material Research Laboratory, Atsugi, Kanagawa (Japan); Kuchitsu, Nobuaki [Independent Administrative Institution National Research Institute for Cultural Properties, Tokyo (Japan)

    2002-11-01

    It is well known that the detection of light elements is difficult using a portable X-ray fluorescence spectrometer with {sup 241}Am (1.85 MBq) as the radiation source. In this study, {sup 55}Fe (3.7 MBq) was used as the radiation source instead of {sup 241}Am, and the beryllium cover of the detector window was thinned in order to increase the sensitivity. As a result, light elements from Si to K could be identified by the investigated method. This method will be effective to specify mineral pigments of mural paintings. (author)

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

    Science.gov (United States)

    Kernstock, Stefan; Koch-Nolte, Friedrich; Mueller-Dieckmann, Jochen; Weiss, Manfred S; Mueller-Dieckmann, Christoph

    2009-05-01

    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 A. 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.

  4. Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

    Science.gov (United States)

    Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893-972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts.

  5. A new detector system for low energy X-ray fluorescence coupled with soft X-ray microscopy: First tests and characterization

    Science.gov (United States)

    Gianoncelli, Alessandra; Bufon, Jernej; Ahangarianabhari, Mahdi; Altissimo, Matteo; Bellutti, Pierluigi; Bertuccio, Giuseppe; Borghes, Roberto; Carrato, Sergio; Cautero, Giuseppe; Fabiani, Sergio; Giacomini, Gabriele; Giuressi, Dario; Kourousias, George; Menk, Ralf Hendrik; Picciotto, Antonino; Piemonte, Claudio; Rachevski, Alexandre; Rashevskaya, Irina; Stolfa, Andrea; Vacchi, Andrea; Zampa, Gianluigi; Zampa, Nicola; Zorzi, Nicola

    2016-04-01

    The last decades have witnessed substantial efforts in the development of several detector technologies for X-ray fluorescence (XRF) applications. In spite of the increasing trend towards performing, cost-effective and reliable XRF systems, detectors for soft X-ray spectroscopy still remain a challenge, requiring further study, engineering and customization in order to yield effective and efficient systems. In this paper we report on the development, first characterization and tests of a novel multielement detector system based on low leakage current silicon drift detectors (SDD) coupled to ultra low noise custom CMOS preamplifiers for synchrotron-based low energy XRF. This new system exhibits the potential for improving the count rate by at least an order of magnitude resulting in ten-fold shorter dwell time at an energy resolution similar to that of single element silicon drift detectors.

  6. A new detector system for low energy X-ray fluorescence coupled with soft X-ray microscopy: First tests and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Gianoncelli, Alessandra, E-mail: alessandra.gianoncelli@elettra.eu [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); Bufon, Jernej [INFN Trieste, Padriciano 99, Trieste 34149 (Italy); Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); University of Trieste, Piazzale Europa 1, Trieste 34127 (Italy); Ahangarianabhari, Mahdi [Politecnico di Milano, Via Anzani 42, Como 22100 (Italy); INFN Milano, Via Celoria 16, Milano 20133 (Italy); Altissimo, Matteo [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); Bellutti, Pierluigi [Fondazione Bruno Kessler, Via Sommarive 18, Trento 38123 (Italy); Bertuccio, Giuseppe [Politecnico di Milano, Via Anzani 42, Como 22100 (Italy); INFN Milano, Via Celoria 16, Milano 20133 (Italy); Borghes, Roberto [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); Carrato, Sergio [University of Trieste, Piazzale Europa 1, Trieste 34127 (Italy); Cautero, Giuseppe [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); INFN Trieste, Padriciano 99, Trieste 34149 (Italy); Fabiani, Sergio [INFN Trieste, Padriciano 99, Trieste 34149 (Italy); Giacomini, Gabriele [Fondazione Bruno Kessler, Via Sommarive 18, Trento 38123 (Italy); Giuressi, Dario [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); INFN Trieste, Padriciano 99, Trieste 34149 (Italy); Kourousias, George [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); Menk, Ralf Hendrik [Elettra-Sincrotrone Trieste S.C.p.A., Strada Statale SS14, km 163.5, Basovizza 34149 (Italy); INFN Trieste, Padriciano 99, Trieste 34149 (Italy); Picciotto, Antonino; Piemonte, Claudio [Fondazione Bruno Kessler, Via Sommarive 18, Trento 38123 (Italy); Rachevski, Alexandre [INFN Trieste, Padriciano 99, Trieste 34149 (Italy); and others

    2016-04-21

    The last decades have witnessed substantial efforts in the development of several detector technologies for X-ray fluorescence (XRF) applications. In spite of the increasing trend towards performing, cost-effective and reliable XRF systems, detectors for soft X-ray spectroscopy still remain a challenge, requiring further study, engineering and customization in order to yield effective and efficient systems. In this paper we report on the development, first characterization and tests of a novel multielement detector system based on low leakage current silicon drift detectors (SDD) coupled to ultra low noise custom CMOS preamplifiers for synchrotron-based low energy XRF. This new system exhibits the potential for improving the count rate by at least an order of magnitude resulting in ten-fold shorter dwell time at an energy resolution similar to that of single element silicon drift detectors.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

  10. Implementation of the phenomenon of total reflection for total reflection X-Ray fluorescence spectrometry technique simulation

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Marcio H. dos; Anjos, Marcelino J. dos; Oliveira, Luis F. de, E-mail: marciohsantos2010@gmail.com, E-mail: bmarcelin@uerj.br, E-mail: clfolive@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Programa de Pos-Graduacao em Fisica; Albuquerque, Marcelo P. de, E-mail: mpalbuquer@gmail.com [Centro Brasileiro de Pesquisas Fisicas (CBPF), Rio de Janeiro, RJ (Brazil). Coordenacao de Atividades Tecnicas

    2015-07-01

    Within the scientific research field, X-ray fluorescence spectrometry is a basic technique for chemical analysis of materials, allowing recognition and study of the elemental nature of a particular sample. With this technique, the researcher uses different devices such as X-ray tubes, radioactive sources, monochromators crystals, capillaries, slits and waveguides, Si-Li detectors and scintillators. Furthermore, one can provide these elements with different arrangements in order to obtain a better configuration. One of the X-ray fluorescence spectrometry variants is the total reflection X-ray fluorescence spectrometry. It is based on the optical phenomenon of total reflection observed when a radiation beam impinges on a surface below a critical angle. Two important characteristics of this technique are to minimize the generation of background derived from the reflector support and allow the radiation interaction with very thin samples (thickness between 100 nm and 15 μm). The goal of the paper is to show the computational modeling of the physical phenomenon of total reflection that enables the implementation of total reflection X-ray fluorescence spectrometry technique through the simulator developed at Institute of Physics of the University of the State of Rio de Janeiro with parallel and distributed processing features. The simulator at hand is already available for implementation of energy dispersive X-ray fluorescence spectrometry. Through it, they are shown three simulations, each based on a particular apparatus: a set of reflectors, a capillary and a waveguide with lucite reflectors. (author)

  11. [Application of the racial algorithm in energy dispersive X-ray fluorescence overlapped spectrum analysis].

    Science.gov (United States)

    Zeng, Guo-Qiang; Luo, Yao-Yao; Ge, Liang-Quan; Zhang, Qing-Xian; Gu, Yi; Cheng, Feng

    2014-02-01

    In the energy dispersive X-ray fluorescence spectrum analysis, scintillation detector such as NaI (Tl) detector usually has a low energy resolution at around 8%. The low energy resolution causes problems in spectral data analysis especially in the high background and low counts condition, it is very limited to strip the overlapped spectrum, and the more overlapping the peaks are, the more difficult to peel the peaks, and the qualitative and quantitative analysis can't be carried out because we can't recognize the peak address and peak area. Based on genetic algorithm and immune algorithm, we build a new racial algorithm which uses the Euclidean distance as the judgment of evolution, the maximum relative error as the iterative criterion to be put into overlapped spectrum analysis, then we use the Gaussian function to simulate different overlapping degrees of the spectrum, and the racial algorithm is used in overlapped peak separation and full spectrum simulation, the peak address deviation is in +/- 3 channels, the peak area deviation is no more than 5%, and it is proven that this method has a good effect in energy dispersive X-ray fluorescence overlapped spectrum analysis.

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

    Science.gov (United States)

    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.

  13. Mapping Metal Elements of Shuangbai Dinosaur Fossil by Synchrotron X-ray Fluorescence Microprobe

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Y.; Qun, Y; Ablett, J

    2008-01-01

    The metal elements mapping of Shuangbai dinosaur fossil, was obtained by synchrotron x-ray fluorescence (SXRF). Eight elements, Ca, Mn, Fe, Cu, Zn, As, Y and Sr were determined. Elements As and Y were detected for the first time in the dinosaur fossil. The data indicated that metal elements are asymmetrical on fossil section. This is different from common minerals. Mapping metals showed that metal element As is few. The dinosaur most likely belongs to natural death. This is different from Zigong dinosaurs which were found dead from poisoning. This method has been used to find that metals Fe and Mn are accrete, and the same is true for Sr and Y. This study indicated that colloid granule Fe and Mn, as well as Sr and Y had opposite electric charges in lithification process of fossils. By this analysis, compound forms can be ascertained. Synchrotron light source x-ray fluorescence is a complementary method that shows mapping of metal elements at the dinosaur fossil, and is rapid, exact and intuitionist. This study shows that dinosaur fossil mineral imaging has a potential in reconstructing the paleoenvironment and ancient geology.

  14. Applications of X-ray fluorescence holography to determine local lattice distortions

    Energy Technology Data Exchange (ETDEWEB)

    Hayashi, Kouichi, E-mail: khayashi@imr.tohoku.ac.jp [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Happo, Naohisa [Graduate School of Information Sciences, Hiroshima City University, Hiroshima 731-3194 (Japan); Hosokawa, Shinya [Department of Physics, Graduate School of Science and Technology, Kumamoto University, Kumamoto 860-8555 (Japan)

    2014-08-15

    Highlights: • We summarized topics of X-ray fluorescence holography focused on the local lattice distortions. • We found details of behaviors of nearest neighbor atoms around dopants. • We found the average distributions of the atoms at the individual sites in mixed crystals. • Distorted and undistorted sires sometimes coexist in a same mixed crystal. - Abstract: X-ray fluorescence holography (XFH) is a method for investigating atomic order up to the medium ranges, and can provide 3D atomic images around specific elements within a radius of nm order. In addition to these characteristics, XFH is sensitive to positional fluctuations of atoms, and therefore it is useful for characterizing the local lattice distortions around specific elements. We have applied XFH to dopants and mixed crystals. We found interesting features in local lattice distortions, such as the displacements of first-neighbor atoms around dopants, far-sighted views of the atomistic fluctuations in mixed crystals, and the coexistence of distorted/undistorted sites in the same material.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lue M, Marco P. [Unidad de Analisis Instrumental, Departamento de Quimica y Suelos, Decanato de Agronomia, Universidad Centro-occidental Lisandro Alvarado, Apartado Postal 4076, Cabudare 3023 (Venezuela)]. E-mail: luemerumarco@yahoo.es; Hernandez-Caraballo, Edwin A. [Instituto Venezolano-Andino para la Investigacion Quimica (IVAIQUIM), Facultad de Ciencias, Universidad de los Andes, Merida 5101 (Venezuela)

    2004-08-31

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

  16. [Determination of major elements in soil from cancer village by X-ray fluorescence spectrometry].

    Science.gov (United States)

    Wei, Zhen-Lin; Li, He; Rui, Yu-Kui

    2008-11-01

    Many social problems arise from environmental pollution, cancer village is one of the many important problems caused by pollution. The authors selected a typical cancer village where 80-100 people died of cancer in the last five years, but there are only a total of 1 200 people in this village. The authors sampled soils from crops-planted areas and detected the major elements by X-ray fluorescence spectrometry. The results showed that the contents of SiO2, TiO2, Al2O3, Fe2O3, MnO, MgO, CaO, Na2O, K2O and P2O5 in soil of this village were 66.05%, 0.66%, 11.37%, 3.93%, 0.075%, 1.97%, 5.47%, 1.90%, 2.11% and 0.20% respectively; with the precision being +/- 0.20%, +/- 0.005%, +/- 0.10%, +/- 0.10%, +/- 0.005%, +/- 0.05%, +/- 0.04%, +/- 0.08%, +/- 0.02% and +/- 0.005% respectively, which showed that X-ray fluorescence spectrometry is a good method.

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

    Science.gov (United States)

    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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

  20. 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

    Energy Technology Data Exchange (ETDEWEB)

    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.)

  1. Promising X-ray fluorescent tests for superconducting tunnel junction detector

    Energy Technology Data Exchange (ETDEWEB)

    Friedrich, Stephan; Robinson, Art

    2001-01-11

    Scientists in the Physical Biosciences Division of the Ernest Orlando Berkeley National Laboratory (Berkeley Lab) studying transition metals in proteins with fluorescence-detected L-edge absorption spectroscopy have found the measurements to be extremely challenging. The difficulty is that the metal centers are present in very dilute concentrations so that their weak fluorescence is often obscured by strong background signals from carbon and oxygen. To solve this problem, the Berkeley group has been working with researchers from the Advanced Detector Group at the Lawrence Livermore National Laboratory on an energy-dispersive superconducting tunnel junction x-ray detector. These devices in principle have the energy resolution needed to reveal the metal signal. The most recent results with the latest version of the detector on Beamline 4.0.1-2 at the Advanced Light Source (ALS) illustrate the promise of the cryogenic detector strategy not only for this application but also for spectroscopy of other types of dilute samples.

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

    Indian Academy of Sciences (India)

    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.

  3. Diffraction enhanced imaging and x-ray fluorescence microtomography for analyzing biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Rocha, H.S.; Pereira, G.R.; Lopes, R.T. [Laboratorio de Instrumentacao Nuclear-COPPE/UFRJ-RJ (Brazil); Anjos, M.J. [Instituto de Fisica-UERJ-RJ (Brazil); Faria, P. [Instituto Nacional do Cancer-INCa-RJ (Brazil); Kellermann, G.; Perez, C.A. [Laboratorio Nacional de Luz Sincrotron-Campinas-SP (Brazil); Tirao, G. [Faculdad de Mat. Astronomia y Fisica (FAMAF), UNC. Cordoba (Argentina); Mazzaro, I. [Laboratorio de Optica de Raios X e Instrumentacao-UFPR-Curitiba-PR (Brazil); Giles, C. [Laboratorio de Cristalografia Aplicada e Raios X-UNICAMP-Campinas-SP (Brazil)

    2007-07-15

    In this work, breast tissue samples were investigated in order to verify the distribution of certain elements by x-ray fluorescence computed tomography (XRFCT) correlated with the characteristics and pathology of each tissue observed by diffraction enhanced imaging (DEI). The DEI system can show details in low attenuation tissues. It is based on the contrast imaging obtained by extinction, diffraction and refraction characteristics and can improve reduction in false positive and false negative diagnoses. XRFCT allows mapping of all elements within the sample, since even a minute fluorescence signal can be detected. DEI imaging techniques revealed the complex structure of the disease, confirmed by the histological section, and showed microstructures in all planes of the sample. The XRFCT showed the distribution of Zn, Cu and Fe at higher concentration. (authors)

  4. Laser 3D micro-manufacturing

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Kouichi Tsuji [Department of Applied Chemistry, Graduate School of Engineering, Osaka City University, 3-3-138 Sugimoto, Sumiyoshi-ku Osaka 558-8585 (Japan); PRESTO-JST - Precursory Research for Embryonic Science and Technology, Japan Science and Technology Agency, 4-1-8 Honcho Kawaguchi, Saitama 332-0012 (Japan); Kazuhiko Nakano [Department of Applied Chemistry, Graduate School of Engineering, Osaka City University, 3-3-138 Sugimoto, Sumiyoshi-ku Osaka 558-8585 (Japan)

    2007-05-15

    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-{mu}m thick Au foil were approximately 90 {mu}m for the x-ray energy of Au L{alpha}. 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)

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

    Science.gov (United States)

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

    2012-09-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Chiari, Giacomo [Getty Conservation Institute, Science Department, Los Angeles, CA (United States); Sarrazin, Philippe [Examinart LLC, Sunnyvale, CA (United States); Heginbotham, Arlen [The J. Paul Getty Museum, Sculpture and Decorative Arts Conservation, Los Angeles, CA (United States)

    2016-11-15

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

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

    Science.gov (United States)

    Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

    2016-11-01

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

  9. Synchrotron X-Ray Fluorescence Microscopy of Gallium in Bladder Tissue following Gallium Maltolate Administration during Urinary Tract Infection

    OpenAIRE

    Ball, Katherine R.; Sampieri, Francesca; Chirino, Manuel; Hamilton, Don L.; Blyth, Robert I. R.; Sham, Tsun-Kong; Dowling, Patricia M.; Thompson, Julie

    2013-01-01

    A mouse model of cystitis caused by uropathogenic Escherichia coli was used to study the distribution of gallium in bladder tissue following oral administration of gallium maltolate during urinary tract infection. The median concentration of gallium in homogenized bladder tissue from infected mice was 1.93 μg/g after daily administration of gallium maltolate for 5 days. Synchrotron X-ray fluorescence imaging and X-ray absorption spectroscopy of bladder sections confirmed that gallium arrived ...

  10. Resonant inelastic scattering in dilute magnetic semiconductors by x-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    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.

  11. Simulated 'On-Line' Wear Metal Analysis of Lubricating Oils by X-Ray Fluorescence Spectroscopy

    Science.gov (United States)

    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.

  12. Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

    Science.gov (United States)

    Nikonow, Wilhelm; Rammlmair, Dieter

    2016-11-01

    Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

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

    Science.gov (United States)

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

    2016-10-01

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

  14. Time-Lapse Observation of Electrolysis of Copper Sulfate with a Full-Field X-ray Fluorescence Imaging Microscope

    Science.gov (United States)

    Ohigashi, Takuji; Aota, Tatsuya; Watanabe, Norio; Takano, Hidekazu; Yokosuka, Hiroki; Aoki, Sadao

    2008-06-01

    The time-lapse observation of the electrodeposition of copper in copper sulfate solution was performed by imaging X-ray fluorescence from the copper deposition. The X-ray fluorescence was directly imaged with a full-field Wolter mirror microscope, which was constructed at the Photon Factory. Controlling the electric current in the solution from 0 to 71.7 µA, the deposition of copper on a Pt cathode was directly observed by imaging its X-ray fluorescence. One exposure time for obtaining an X-ray fluorescence image was 80 s. Then, it was 17 min later from the beginning of the electrolysis when the X-ray fluorescence image of the electrodeposition is observed for the first time. At this exposure time, the detection limit of the mass of copper was estimated to be 0.60 pg/image, which was calculated using test samples of 1.00×10-3-1.00 mol/l copper sulfate solutions.

  15. Detection of Fingerprints Based on Elemental Composition Using Micro-X-Ray Fluorescence.

    Energy Technology Data Exchange (ETDEWEB)

    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

  16. Toward chromium speciation in solids using wavelength dispersive X-ray fluorescence spectrometry Cr Kβ lines.

    Science.gov (United States)

    Malherbe, J; Claverie, F

    2013-04-22

    The determination of chromium speciation in solid samples is critical for environmental and industrial purposes. Several analytical methods exist to perform such a determination either directly in solid state or liquid state after an extraction step, each of them having some limitations. In this study, the use of a high-resolution wavelength-dispersive X-ray fluorescence spectrometer to determine and quantify chromium species is investigated by looking at the differences in the Kβ transition profiles between Cr(0), Cr(III) and Cr(VI) compounds. Three different approaches were tested and compared to determine the Cr(VI) fraction of known mixtures: relative height and peak fitting using calibration mixtures, partial least square regression (PLS) of pure compounds, and principal component regression (PCR) of pure compounds. The accuracy of these methods was found to be about the same with an average relative error in the range of 15%. However, PLS and PCR can be easily implemented in an automated way contrary to peak fitting which can be sometimes perceived as analyst-dependant. Another advantage of using PLS and PCR is that information concerning the other oxidation states present in the sample can be retrieved. Finally, PLS and the peak height approach can be used up to 0.5% total chromium which make the XRF an alternative technique to X-ray induced photoelectron spectroscopy (XPS) for chromium speciation in solid state.

  17. Modeling of x-ray fluorescence using MCNPX and Geant4

    Energy Technology Data Exchange (ETDEWEB)

    Rajasingam, Akshayan [Los Alamos National Laboratory; Hoover, Andrew S [Los Alamos National Laboratory; Fensin, Michael L [Los Alamos National Laboratory; Tobin, Stephen J [Los Alamos National Laboratory

    2009-01-01

    X-Ray Fluorescence (XRF) is one of thirteen non-destructive assay techniques being researched for the purpose of quantifying the Pu mass in used fuel assemblies. The modeling portion of this research will be conducted with the MCNPX transport code. The research presented here was undertaken to test the capability of MCNPX so that it can be used to benchmark measurements made at the ORNL and to give confidence in the application of MCNPX as a predictive tool of the expected capability of XRF in the context of used fuel assemblies. The main focus of this paper is a code-to-code comparison between MCNPX and Geant4 code. Since XRF in used fuel is driven by photon emission and beta decay of fission fragments, both terms were independently researched. Simple cases and used fuel cases were modeled for both source terms. In order to prepare for benchmarking to experiments, it was necessary to determine the relative significance of the various fission fragments for producing X-rays.

  18. 3D Imaging of Transition Metals in the Zebrafish Embryo by X-ray Fluorescence Microtomography

    Science.gov (United States)

    Bourassa, Daisy; Gleber, Sophie-Charlotte; Vogt, Stefan; Yi, Hong; Will, Fabian; Richter, Heiko; Shin, Chong Hyun; Fahrni, Christoph J.

    2014-01-01

    Synchrotron X-ray fluorescence (SXRF) microtomography has emerged as a powerful technique for the 3D visualization of the elemental distribution in biological samples. The mechanical stability, both of the instrument and the specimen, is paramount when acquiring tomographic projection series. By combining the progressive lowering of temperature method (PLT) with femtosecond laser sectioning, we were able to embed, excise, and preserve a zebrafish embryo at 24 hours post fertilization in an X-ray compatible, transparent resin for tomographic elemental imaging. Based on a data set comprised of 60 projections, acquired with a step size of 2 μm during 100 hours of beam time, we reconstructed the 3D distribution of zinc, iron, and copper using the iterative maximum likelihood expectation maximization (MLEM) reconstruction algorithm. The volumetric elemental maps, which entail over 124 million individual voxels for each transition metal, revealed distinct elemental distributions that could be correlated with characteristic anatomical features at this stage of embryonic development. PMID:24992831

  19. Radiography and X-ray fluorescence used to analyze cultural and artistic artifacts

    Energy Technology Data Exchange (ETDEWEB)

    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)

  20. Fundamental parameter based quantification algorithm for confocal nano-X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Schoonjans, Tom, E-mail: Tom.Schoonjans@UGent.be [X-ray Microspectroscopy and Imaging Research Group (XMI), Department of Analytical Chemistry, Ghent University, Krijgslaan 281 S12, B-9000 Ghent (Belgium); Silversmit, Geert; Vekemans, Bart [X-ray Microspectroscopy and Imaging Research Group (XMI), Department of Analytical Chemistry, Ghent University, Krijgslaan 281 S12, B-9000 Ghent (Belgium); Schmitz, Sylvia [Geosciences Institute/Mineralogy, Goethe University Frankfurt, Altenhoeferallee 1, D-60438 Frankfurt (Germany); Burghammer, Manfred; Riekel, Christian [ESRF, 6 rue Jules Horowitz, BP220, F-38043 Grenoble Cedex (France); Brenker, Frank E. [Geosciences Institute/Mineralogy, Goethe University Frankfurt, Altenhoeferallee 1, D-60438 Frankfurt (Germany); Vincze, Laszlo, E-mail: Laszlo.Vincze@UGent.be [X-ray Microspectroscopy and Imaging Research Group (XMI), Department of Analytical Chemistry, Ghent University, Krijgslaan 281 S12, B-9000 Ghent (Belgium)

    2012-01-15

    A new method for the quantification of X-ray fluorescence (XRF) was derived based on the fundamental parameter method (FPM). The FPM equations were adapted to accommodate the special case of confocal nano-XRF, i.e. X-ray nano-beam excitation coupled with confocal detection, taking into account the special characteristics of the detector channel polycapillary. A thorough error estimation algorithm based on the Monte Carlo method was applied, producing a detailed analysis of the uncertainties of the quantification results. The new FPM algorithm was applied on confocal nano-XRF data obtained from cometary dust returned by NASA's Stardust mission, recorded at beamline ID13 of the European Synchrotron Radiation Facility. - Highlights: Black-Right-Pointing-Pointer A new method for the quantification of confocal XRF is presented. Black-Right-Pointing-Pointer The quantification is based on the fundamental parameter method (FPM). Black-Right-Pointing-Pointer The new FPM algorithm was applied for the analysis of unique cometary dust particles. Black-Right-Pointing-Pointer The cometary particles were returned by NASA's Stardust mission in 2006. Black-Right-Pointing-Pointer Error estimation is based on the Monte Carlo method.

  1. Investigation of X-ray fluorescence computed tomography (XFCT) and K-edge imaging.

    Science.gov (United States)

    Bazalova, Magdalena; Kuang, Yu; Pratx, Guillem; Xing, Lei

    2012-08-01

    This work provides a comprehensive Monte Carlo study of X-ray fluorescence computed tomography (XFCT) and K-edge imaging system, including the system design, the influence of various imaging components, the sensitivity and resolution under various conditions. We modified the widely used EGSnrc/DOSXYZnrc code to simulate XFCT images of two acrylic phantoms loaded with various concentrations of gold nanoparticles and Cisplatin for a number of XFCT geometries. In particular, reconstructed signal as a function of the width of the detector ring, its angular coverage and energy resolution were studied. We found that XFCT imaging sensitivity of the modeled systems consisting of a conventional X-ray tube and a full 2-cm-wide energy-resolving detector ring was 0.061% and 0.042% for gold nanoparticles and Cisplatin, respectively, for a dose of ∼ 10 cGy. Contrast-to-noise ratio (CNR) of XFCT images of the simulated acrylic phantoms was higher than that of transmission K-edge images for contrast concentrations below 0.4%.

  2. Spectrum reconstruction method based on the detector response model calibrated by x-ray fluorescence

    Science.gov (United States)

    Li, Ruizhe; Li, Liang; Chen, Zhiqiang

    2017-02-01

    Accurate estimation of distortion-free spectra is important but difficult in various applications, especially for spectral computed tomography. Two key problems must be solved to reconstruct the incident spectrum. One is the acquisition of the detector energy response. It can be calculated by Monte Carlo simulation, which requires detailed modeling of the detector system and a high computational power. It can also be acquired by establishing a parametric response model and be calibrated using monochromatic x-ray sources, such as synchrotron sources or radioactive isotopes. However, these monochromatic sources are difficult to obtain. Inspired by x-ray fluorescence (XRF) spectrum modeling, we propose a feasible method to obtain the detector energy response based on an optimized parametric model for CdZnTe or CdTe detectors. The other key problem is the reconstruction of the incident spectrum with the detector response. Directly obtaining an accurate solution from noisy data is difficult because the reconstruction problem is severely ill-posed. Different from the existing spectrum stripping method, a maximum likelihood-expectation maximization iterative algorithm is developed based on the Poisson noise model of the system. Simulation and experiment results show that our method is effective for spectrum reconstruction and markedly increases the accuracy of XRF spectra compared with the spectrum stripping method. The applicability of the proposed method is discussed, and promising results are presented.

  3. Tibial lead determination by 99Tcm radiopharmaceutical x-ray fluorescence.

    Science.gov (United States)

    Mountford, P J; Green, S; Bradley, D A; Lewis, A D; Morgan, W D

    1994-04-01

    The feasibility of measuring tibial lead concentration by x-ray fluorescence with an internal 99Tcm labelled bone-seeking radiopharmaceutical was investigated using phantoms containing known values of lead concentration and 99Tcm activity. The minimum detectable concentration (MDC) at two standard deviations based on the counts in the Kalpha1 peak of 10.9 microg Pb ml(-1) was estimated to correspond to an MDC for an individual within a range of approximately 8-15 microg Pb (g bone mineral)(-1) if the counts from all four K x-ray peaks were included. Due to its much greater dose compared to an external source, the MDC of this internal source technique would have to be reduced before it could be used for measurements of occupationally or environmentally exposed individuals other than as an adjunct for a patient undergoing a bone scan. Methods of achieving such a reduction include increasing the acquisition time and the number of HPGE detectors, and optimizing the design of their collimators.

  4. Synchrotron-based X-ray fluorescence imaging and elemental mapping from biological samples

    Energy Technology Data Exchange (ETDEWEB)

    D Rao; M Swapna; R Cesareo; A Brunetti; T Akatsuka; T Yuasa; T Takeda; G Gigante

    2011-12-31

    The present study utilized the new hard X-ray microspectroscopy beamline facility, X27A, available at NSLS, BNL, USA, for elemental mapping. This facility provided the primary beam in a small spot of the order of {approx}10 {mu}m, for focussing. With this spatial resolution and high flux throughput, the synchrotron-based X-ray fluorescent intensities for Mn, Fe, Zn, Cr, Ti and Cu were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. The sample is scanned in a 'step-and-repeat' mode for fast elemental mapping measurements and generated elemental maps at 8, 10 and 12 keV, from a small animal shell (snail). The accumulated trace elements, from these biological samples, in small areas have been identified. Analysis of the small areas will be better suited to establish the physiology of metals in specific structures like small animal shell and the distribution of other elements.

  5. Standard test methods for chemical analysis of ceramic whiteware materials using wavelength dispersive X-Ray fluorescence spectrometry

    CERN Document Server

    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...

  6. Elemental Analysis of Variably Contaminated Cremains Using X-ray Fluorescence Spectrometry.

    Science.gov (United States)

    Gilpin, Megan; Christensen, Angi M

    2015-07-01

    Analyzing and identifying skeletal remains becomes increasingly difficult when remains have been cremated, especially in cases where the cremated material may have been intentionally contaminated with nonskeletal material. This study examined the potential of X-ray fluorescence spectrometry (XRF) to detect the presence of nonskeletal contaminants in samples of cremains. Eleven samples of cremains were variably combined with concrete mix and analyzed using XRF. Photon counts of elements in each sample were analyzed, and the coefficient of determination (R(2)) using unweighted linear regression as a function of percent cremains was calculated. Results showed that with changes in the proportion of skeletal material and contaminant, there were significant (R(2) > 0.90) changes in detected levels of phosphorus, potassium, zinc, aluminum, and sulfur. The use of XRF is concluded to be a valid approach in the identification of the presence of nonskeletal material in potentially contaminated cremains.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  8. Mapping metals in Parkinson's and normal brain using rapid-scanning x-ray fluorescence

    Science.gov (United States)

    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.

  9. In-situ assessment of metal contamination via portable X-ray fluorescence spectroscopy: Zlatna, Romania.

    Science.gov (United States)

    Weindorf, David C; Paulette, Laura; Man, Titus

    2013-11-01

    Zlatna, Romania is the site of longtime mining/smelting operations which have resulted in widespread metal pollution of the entire area. Previous studies have documented the contamination using traditional methods involving soil sample collection, digestion, and quantification via inductively coupled plasma atomic emission spectroscopy or atomic absorption. However, field portable X-ray fluorescence spectroscopy (PXRF) can accurately quantify contamination in-situ, in seconds. A PXRF spectrometer was used to scan 69 soil samples in Zlatna across multiple land use types. Each site was georeferenced with data inputted into a geographic information system for high resolution spatial interpolations. These models were laid over contemporary aerial imagery to evaluate the extent of pollution on an individual elemental basis. Pb, As, Co, Cu, and Cd exceeded governmental action limits in >50% of the sites scanned. The use of georeferenced PXRF data offers a powerful new tool for in-situ assessment of contaminated soils.

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

    Science.gov (United States)

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

    1986-01-01

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

  11. Analysis of photographs and photo-paintings by energy-dispersive X-ray fluorescence spectroscopy

    Science.gov (United States)

    Neiva, Augusto Camara; Marcondes, Marli A.; Pinto, Herbert Prince Favero; Almeida, Paula Aline Durães

    2014-02-01

    A collection of Brazilian family photographs and photo-paintings from the beginning of the XX Century was analyzed by portable EDXRF (Energy-Dispersive X-Ray Fluorescence) spectroscopy. The spectrometer uses a Si-drift Amptek detector and an Oxford Cr-tube or an Oxford W-tube. For every region under analysis, spectra obtained with the W-tube were used to detect all the elements above Al, while the Cr-tube was used to obtain more accurate results for elements between Al and V. Thirty nine elements were identified in the photos, and the origin of the most important ones was discussed. These results can be used for cataloging, preservation and restoring procedures.

  12. [Analysis of 14 elements for Jinhua bergamot by X-ray fluorescence spectrometry and elemental analyser].

    Science.gov (United States)

    Wang, Zhi-gang; Yu, Hong-mei

    2012-01-01

    The content of the elements C, H, O and N in Jinhua bergamot was analysed by using Vario III elemental analyser, the bergamot sample was scanned by using X-ray fluorescence spectrometer with PW2400 wavelength dispersion, and the content of the elements Mg, Al, P, S, Cl, K, Ca, Mn, Fe and Sr was analysed by using IQ+ analytical method. It turned out that the result is more ideal if the content of the elements C, H, O and N is processed as fix phase, and the analytical result is more ideal if, to prevent the sample skin from coming off, the sample is wrapped with mylar film with the film coefficient adjusted.

  13. 100-OL-1 Operable Unit Field Portable X-Ray Fluorescence (XRF) Analyzer Pilot Study Plans

    Energy Technology Data Exchange (ETDEWEB)

    Bunn, Amoret L. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Fritz, Brad G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Wellman, Dawn M. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2014-07-01

    A pilot study is being conducted to support the approval of the Remedial Investigation/Feasibility Study (RI/FS) Work Plan to evaluate the 100-OL-1 Operable Unit (OU) pre-Hanford orchard lands. Based on comments received by the U.S. Environmental Protection Agency (EPA) and Washington State Department of Ecology, the pilot study will evaluate the use of field portable X-ray fluorescence (XRF) spectrometry measurements for evaluating lead and arsenic concentrations on the soil surface as an indicator of past use of lead arsenate pesticide residue in the OU. The work will be performed in the field during the summer of 2014, and assist in the planning for the characterization activities in the RI/FS.

  14. [Progress in application of microbeam X-ray fluorescence spectroscopy in forensic science].

    Science.gov (United States)

    Su, Hui-Fang; Liu, Chao; Hu, Sun-Lin; Wang, Song-Cai; Sun, Li-Min; Huang, Wei; Zhang, Xiao-Ting; Li, Shuang-Lin

    2013-02-01

    Microbeam X-ray fluorescence (micro-XRF) spectrometry has been raised as an analytical technique of microbeam during the recent years. With its advantages of high sensitivity, small sample requirement, high testing accuracy and non-destruction, the technique is widely utilized in forensic science. This review bases on recent researches at home and abroad, describes its applications including identification of gunshot residue, visualization of fingerprints, discrimination of drug source, production process, and other material evidences of analysis in crime scene. Thanks to the advances in technology, intelligent and portable micro-XRF equipment has appeared to be applied. It is believed that it may be more popular and frequent in administration of forensic science in the near future.

  15. Trace element distribution in human teeth by x-ray fluorescence spectrometry and multivariate statistical analysis

    CERN Document Server

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-01

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

  17. Identifying metalloproteins through X-ray fluorescence mapping and mass spectrometry.

    Science.gov (United States)

    Raimunda, Daniel; Khare, Tripti; Giometti, Carol; Vogt, Stefan; Argüello, José M; Finney, Lydia

    2012-08-01

    Metals are critical and dynamic components of biochemistry. To understand their roles, we greatly need tools to identify the ligands that bind them within the complexity of natural systems. This work describes the development of methods that not only detect and distinguish metals, but also characterize the proteins that bind them. We describe an approach to expose, identify and quantify metalloproteins in complex mixtures by sequential non-denaturing 2D-gel electrophoresis (2D GE)/X-ray Fluorescence (XRF) and tandem mass spectrometry (MS/MS) in the same spot of a sample. We first apply the development of 2D GE/XRF to Shewanella oneidensis MR-1, a well-studied system, and verify our electrophoretic approach. Then, we identified a novel periplasmic zinc protein in Pseudomonas aeruginosa PAO1 through 2D GE/XRF followed by MS/MS. The identity and function of this protein was verified through a gene mutation experiment.

  18. Analytic Comparison between X-ray Fluorescence CT and K-edge CT

    CERN Document Server

    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.

  19. Detection of visible and latent fingerprints using micro-X-ray fluorescence elemental imaging.

    Science.gov (United States)

    Worley, Christopher G; Wiltshire, Sara S; Miller, Thomasin C; Havrilla, George J; Majidi, Vahid

    2006-01-01

    Using micro-X-ray fluorescence (MXRF), a novel means of detecting fingerprints was examined in which the prints were imaged based on their elemental composition. MXRF is a nondestructive technique. Although this method requires a priori knowledge about the approximate location of a print, it offers a new and complementary means for detecting fingerprints that are also left pristine for further analysis (including potential DNA extraction) or archiving purposes. Sebaceous fingerprints and those made after perspiring were detected based on elements such as potassium and chlorine present in the print residue. Unique prints were also detected including those containing lotion, saliva, banana, or sunscreen. This proof-of-concept study demonstrates the potential for visualizing fingerprints by MXRF on surfaces that can be problematic using current methods.

  20. X-Ray Fluorescence to Determine Zn in Bolivian Children using Hair Samples

    Energy Technology Data Exchange (ETDEWEB)

    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.

  1. X-ray spectra of Hercules X-1. I - Iron line fluorescence from a subrelativistic shell

    Science.gov (United States)

    Pravdo, S. H.; Becker, R. H.; Boldt, E. A.; Holt, S. S.; Serlemitsos, P. J.; Swank, J. H.

    1977-01-01

    The X-ray spectrum of Her X-1 was observed in the energy range from 2 to 24 keV from August 29 to September 3, 1975. Emission features are observed near the K-alpha iron-line energy which exhibit both broadening and a double line structure. The total luminosity in these features is about 4 by 10 to the 35th power ergs/s. Iron line fluorescence from an opaque cool (not exceeding 1 million K) shell of material at the Alfven surface provides the necessary luminosity in this feature. The double line structure and the line energy width can be due to Doppler shifts if the shell is forced to corotate with the pulsar at a radius of at least 800 million cm. Implications of this model regarding physical conditions near Her X-1 are discussed.

  2. 100-OL-1 Operable Unit Field Portable X-Ray Fluorescence (XRF) Analyzer Pilot Study Plans

    Energy Technology Data Exchange (ETDEWEB)

    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.

  3. Calcium and Phosphorus Detection Using Benchtop Versus Handheld X-ray Fluorescence Spectrometers.

    Science.gov (United States)

    Kuzel, Aaron R; Christensen, Angi M; Marvin, Susan M

    2016-01-01

    Elemental analysis of calcium (Ca) and phosphorus (P) has been shown to be useful in differentiating skeletal and nonskeletal material. X-ray fluorescence spectrometry (XRF) is an attractive, nondestructive technique for forensic anthropologists, and the development of portable XRF instrumentation is promising for field applications. This study examines the performance of handheld XRF instrumentation operated in air compared to a traditional benchtop XRF device that has the ability to control the analysis atmosphere. Both instruments can be used to effectively distinguish skeletal from nonskeletal remains. However, as the measurement atmosphere affects detection levels for calcium and phosphorus, Ca/P ratios obtained from the instruments and analysis conditions were found to differ significantly, with analyses conducted in air showing significantly lower phosphorus detection. Consequently, comparison of Ca/P ratios to conclude skeletal versus nonskeletal origin must be based on data collected under similar analysis conditions.

  4. Performance of a Borehole X-ray Fluorescence Spectrometer for Planetary Exploration

    Science.gov (United States)

    Kelliher, Warren C.; Carlberg, Ingrid A.; Elam, W. T.; Willard-Schmoe, Ella

    2008-01-01

    We have designed and constructed a borehole X-ray Fluorescence Spectrometer (XRFS) as part of the Mars Subsurface Access program [1]. It can be used to determine the composition of the Mars regolith at various depths by insertion into a pre-drilled borehole. The primary requirements and performance metrics for the instrument are to obtain parts-per-million (ppm) lower limits of detection over a wide range of elements in the periodic table (Magnesium to Lead). Power consumption during data collection was also measured. The prototype instrument is complete and preliminary testing has been performed. Terrestrial soil Standard Reference Materials were used as the test samples. Detection limits were about 10 weight ppm for most elements, with light elements being higher, up to 1.4 weight percent for magnesium. Power consumption (excluding ground support components) was 12 watts.

  5. High resolution X-ray fluorescence imaging for a microbeam radiation therapy treatment planning system

    Science.gov (United States)

    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.

  6. Identifying microbial habitats in soil using quantum dots and x-ray fluorescence microtomography

    Science.gov (United States)

    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.

  7. Uranium and plutonium solution assays by transmission-corrected x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    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.

  8. Quantitative micro x-ray fluorescence analyses without reference standard material; Referenzprobenfreie quantitative Mikro-Roentgenfluoreszenzanalyse

    Energy Technology Data Exchange (ETDEWEB)

    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

  9. X-ray fluorescence imaging reveals subcellular biometal disturbances in a childhood neurodegenerative disorder.

    Science.gov (United States)

    Grubman, A; James, S A; James, J; Duncan, C; Volitakis, I; Hickey, J L; Crouch, P J; Donnelly, P S; Kanninen, K M; Liddell, J R; Cotman, S L; de Jonge; White, A R

    2014-06-01

    Biometals such as zinc, iron, copper and calcium play key roles in diverse physiological processes in the brain, but can be toxic in excess. A hallmark of neurodegeneration is a failure of homeostatic mechanisms controlling the concentration and distribution of these elements, resulting in overload, deficiency or mislocalization. A major roadblock to understanding the impact of altered biometal homeostasis in neurodegenerative disease is the lack of rapid, specific and sensitive techniques capable of providing quantitative subcellular information on biometal homeostasis in situ. Recent advances in X-ray fluorescence detectors have provided an opportunity to rapidly measure biometal content at subcellular resolution in cell populations using X-ray Fluorescence Microscopy (XFM). We applied this approach to investigate subcellular biometal homeostasis in a cerebellar cell line isolated from a natural mouse model of a childhood neurodegenerative disorder, the CLN6 form of neuronal ceroid lipofuscinosis, commonly known as Batten disease. Despite no global changes to whole cell concentrations of zinc or calcium, XFM revealed significant subcellular mislocalization of these important biological second messengers in cerebellar Cln6(nclf) (CbCln6(nclf) ) cells. XFM revealed that nuclear-to-cytoplasmic trafficking of zinc was severely perturbed in diseased cells and the subcellular distribution of calcium was drastically altered in CbCln6(nclf) cells. Subtle differences in the zinc K-edge X-ray Absorption Near Edge Structure (XANES) spectra of control and CbCln6(nclf) cells suggested that impaired zinc homeostasis may be associated with an altered ligand set in CbCln6(nclf) cells. Importantly, a zinc-complex, Zn(II)(atsm), restored the nuclear-to-cytoplasmic zinc ratios in CbCln6(nclf) cells via nuclear zinc delivery, and restored the relationship between subcellular zinc and calcium levels to that observed in healthy control cells. Zn(II)(atsm) treatment also resulted in a

  10. Characterization of X-ray polycapillary optics by LiF crystal radiation detectors through confocal fluorescence microscopy

    Science.gov (United States)

    Bonfigli, Francesca; Hampai, Dariush; Dabagov, Sultan B.; Montereali, Rosa Maria

    2016-08-01

    Solid-state radiation imaging detectors based on photoluminescent colour centres in lithium fluoride (LiF) crystals have been successfully tested for both advanced 2D and 3D characterizations of X-ray polycapillary optics by a table-top laboratory system. Polycapillary optics can control X-ray beams propagation and allows obtaining quasi-parallel beam (half-lens) or focused beams (full-lens). The combination of a fine-focused micro X-ray tube and a polycapillary lens can provide the high intensity radiation fluxes that are necessary for high resolution X-ray imaging. In this paper we present novel results about advanced characterization of these complex optics by 2D as well as 3D confocal laser fluorescence microscopy of X-ray irradiated LiF crystal detectors. Two dimensional high spatial resolution images on a wide field of view of transmitted X-rays through a semi-lens and 3D direct inspection of the coloured volumes produced in LiF crystals by both focused and parallel X-ray beam transmitted by a full and a semi-lens, respectively, as well as their 3D reconstructions were obtained. The results show that the photoluminescent colour centres volume in LiF crystals combined with an optical sectioning reading system provide information about tomography of transmitted X-ray beams by policapillary optics in a single exposure process. For the first time, the use of LiF crystal plates as versatile radiation imaging luminescent detectors have been used to characterize the operation of polycapillary optics as X-ray lens, in focusing and parallel mode.

  11. 2D/3D cryo x-ray fluorescence imaging at the bionanoprobe at the advanced photon source

    Energy Technology Data Exchange (ETDEWEB)

    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.

  12. X-ray nanoprobes and diffraction-limited storage rings: opportunities and challenges of fluorescence tomography of biological specimens

    Energy Technology Data Exchange (ETDEWEB)

    Jonge, Martin D. de, E-mail: martin.dejonge@synchrotron.org.au [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia); Ryan, Christopher G. [CSIRO Earth Science and Research Engineering, Clayton, Victoria 3168 (Australia); Jacobsen, Chris J. [Advanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Department of Physics, Chemistry of Life Processes Institute, Northwestern University, 2170 Campus Drive, Evanston, IL 60208 (United States); Chemistry of Life Processes Institute, Northwestern University, 2170 Campus Drive, Evanston, IL 60208 (United States)

    2014-08-27

    Nanoscale X-ray scanning microscopes, or X-ray nanoprobes, will benefit greatly from diffraction-limited storage rings. Here the requirements for nanoscale fluorescence tomography are explored to gain insight into the scientific opportunities and technical challenges that such sources offer. X-ray nanoprobes require coherent illumination to achieve optic-limited resolution, and so will benefit directly from diffraction-limited storage rings. Here, the example of high-resolution X-ray fluorescence tomography is focused on as one of the most voracious demanders of coherent photons, since the detected signal is only a small fraction of the incident flux. Alternative schemes are considered for beam delivery, sample scanning and detectors. One must consider as well the steps before and after the X-ray experiment: sample preparation and examination conditions, and analysis complexity due to minimum dose requirements and self-absorption. By understanding the requirements and opportunities for nanoscale fluorescence tomography, one gains insight into the R&D challenges in optics and instrumentation needed to fully exploit the source advances that diffraction-limited storage rings offer.

  13. Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

    Energy Technology Data Exchange (ETDEWEB)

    Blagoev, K., E-mail: kblagoev@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Grozeva, M., E-mail: margo@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Malcheva, G., E-mail: bobcheva@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Neykova, S., E-mail: sevdalinaneikova@abv.bg [National Institute of Archaeology with Museum, Bulgarian Academy of Sciences, 2 Saborna, 1000 Sofia (Bulgaria)

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893–972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts. - Highlights: ► LIBS, XRF and XRD analyses of medieval white-clay ceramic tiles fragments are done. ► Different elements and phases, presented in the ceramics fragments were determined. ► Differences in the tiles' raw material mineral composition are found. ► Information of the tiles' production process and the raw clay deposits is obtained.

  14. Iron speciation in human cancer cells by K-edge total reflection X-ray fluorescence-X-ray absorption near edge structure analysis

    Energy Technology Data Exchange (ETDEWEB)

    Polgari, Zs. [Eoetvoes Lorand University, Institute of Chemistry, Department of Analytical Chemistry, Laboratory of Environmental Chemistry and Bioanalytics, P.O. Box 32, H-1518, Budapest (Hungary); Meirer, F. [Institute of Atomic and Subatomic Physics, Vienna University of Technology, Vienna (Austria); MiNALab, CMM-irst, Fondazione Bruno Kessler, Povo, Trento (Italy); Sasamori, S.; Ingerle, D. [Institute of Atomic and Subatomic Physics, Vienna University of Technology, Vienna (Austria); Pepponi, G. [MiNALab, CMM-irst, Fondazione Bruno Kessler, Povo, Trento (Italy); Streli, C. [Institute of Atomic and Subatomic Physics, Vienna University of Technology, Vienna (Austria); Rickers, K. [Hamburger Synchrotronstrahlungslabor at DESY, Hamburg (Germany); Reti, A.; Budai, B. [Department of Clinical Research, National Institute of Oncology, Budapest (Hungary); Szoboszlai, N. [Eoetvoes Lorand University, Institute of Chemistry, Department of Analytical Chemistry, Laboratory of Environmental Chemistry and Bioanalytics, P.O. Box 32, H-1518, Budapest (Hungary); Zaray, G., E-mail: zaray@ludens.elte.hu [Eoetvoes Lorand University, Institute of Chemistry, Department of Analytical Chemistry, Laboratory of Environmental Chemistry and Bioanalytics, P.O. Box 32, H-1518, Budapest (Hungary)

    2011-03-15

    X-ray absorption near edge structure (XANES) analysis in combination with synchrotron radiation induced total reflection X-ray fluorescence (SR-TXRF) acquisition was used to determine the oxidation state of Fe in human cancer cells and simultaneously their elemental composition by applying a simple sample preparation procedure consisting of pipetting the cell suspension onto the quartz reflectors. XANES spectra of several inorganic and organic iron compounds were recorded and compared to that of different cell lines. The XANES spectra of cells, independently from the phase of cell growth and cell type were very similar to that of ferritin, the main Fe store within the cell. The spectra obtained after CoCl{sub 2} or NiCl{sub 2} treatment, which could mimic a hypoxic state of cells, did not differ noticeably from that of the ferritin standard. After 5-fluorouracil administration, which could also induce an oxidative-stress in cells, the absorption edge position was shifted toward higher energies representing a higher oxidation state of Fe. Intense treatment with antimycin A, which inhibits electron transfer in the respiratory chain, resulted in minor changes in the spectrum, resembling rather the N-donor Fe-{alpha},{alpha}'-dipyridyl complex at the oxidation energy of Fe(III), than ferritin. The incorporation of Co and Ni in the cells was followed by SR-TXRF measurements.

  15. X-Ray Diffraction (XRD and X-Ray Fluorescence (XRF Analysis of Proto-historic Votive Tablets from Chawas Cave, Hulu Kelantan, Malaysia

    Directory of Open Access Journals (Sweden)

    Zuliskandar Ramli

    2014-02-01

    Full Text Available This research was conducted to determine the origin of votive tablets found in prehistoric and proto-historic site of Chawas Cave in Hulu Kelantan. The votive tablets found in Chawas Cave showed several Buddhist images which are associated with the Srivijaya Kingdom which existed from 7th century AD until 12th century AD. To determine if the votive tablets were produced by communities that lived in Hulu Kelantan, hence the study of the chemical composition of the votive tablets should be carried out. Two techniques were employed in this research, namely the X-Ray Diffraction (XRD and X-Ray Fluorescence (XRF techniques. The techniques will determine the mineral content as well as the major and trace element content of the votive tablets. Analysis showed that all the votive tablet samples have mineral known as clinochlore. Clinochlore is one of the chlorites, namely a group of phyllosilicate minerals. Chlorite is commonly found in igneous rocks as an alteration product of mafic minerals such as pyroxene, amphibole and biotite. The votive tablets were found in a cave which consisted of limestone cave formation and it showed that the votive tablets were not produced by the local community of Hulu Kelantan. Major elements also showed that the chemical composition of the votive tablets is not similar to the composition of clay samples taken from several rivers in Hulu Kelantan.

  16. Rapid and reliable diagnosis of Wilson disease using X-ray fluorescence.

    Science.gov (United States)

    Kaščáková, Slávka; Kewish, Cameron M; Rouzière, Stéphan; Schmitt, Françoise; Sobesky, Rodolphe; Poupon, Joël; Sandt, Christophe; Francou, Bruno; Somogyi, Andrea; Samuel, Didier; Jacquemin, Emmanuel; Dubart-Kupperschmitt, Anne; Nguyen, Tuan Huy; Bazin, Dominique; Duclos-Vallée, Jean-Charles; Guettier, Catherine; Le Naour, François

    2016-07-01

    Wilson's disease (WD) is a rare autosomal recessive disease due to mutations of the gene encoding the copper-transporter ATP7B. The diagnosis is hampered by the variability of symptoms induced by copper accumulation, the inconstancy of the pathognomonic signs and the absence of a reliable diagnostic test. We investigated the diagnostic potential of X-ray fluorescence (XRF) that allows quantitative analysis of multiple elements. Studies were performed on animal models using Wistar rats (n = 10) and Long Evans Cinnamon (LEC) rats (n = 11), and on human samples including normal livers (n = 10), alcohol cirrhosis (n = 8), haemochromatosis (n = 10), cholestasis (n = 6) and WD (n = 22). XRF experiments were first performed using synchrotron radiation to address the elemental composition at the cellular level. High-resolution mapping of tissue sections allowed measurement of the intensity and the distribution of copper, iron and zinc while preserving the morphology. Investigations were further conducted using a laboratory X-ray source for irradiating whole pieces of tissue. The sensitivity of XRF was highlighted by the discrimination of LEC rats from wild type even under a regimen using copper deficient food. XRF on whole formalin-fixed paraffin embedded needle biopsies allowed profiling of the elements in a few minutes. The intensity of copper related to iron and zinc significantly discriminated WD from other genetic or chronic liver diseases with 97.6% specificity and 100% sensitivity. This study established a definite diagnosis of Wilson's disease based on XRF. This rapid and versatile method can be easily implemented in a clinical setting.

  17. Portable x-ray fluorescence for the analysis of chromium in nail and nail clippings.

    Science.gov (United States)

    Fleming, David E B; Ware, Chris S

    2017-03-01

    Assessment of chromium content in human nail or nail clippings could serve as an effective biomarker of chromium status. The feasibility of a new portable x-ray fluorescence (XRF) approach to chromium measurement was investigated through analysis of nail and nail clipping phantoms. Five measurements of 180s (real time) duration were first performed on six whole nail phantoms having chromium concentrations of 0, 2, 5, 10, 15, and 20µg/g. Using nail clippers, these phantoms were then converted to nail clippings, and assembled into different mass groups of 20, 40, 60, 80, and 100mg for additional measurements. The amplitude of the chromium Kα characteristic x-ray energy peak was examined as a function of phantom concentration for all measurement conditions to create a series of calibration lines. The minimum detection limit (MDL) for chromium was also calculated for each case. The chromium MDL determined from the whole nail intact phantoms was 0.88±0.03µg/g. For the clipping phantoms, the MDL ranged from 1.2 to 3.3µg/g, depending on the mass group analyzed. For the 40mg clipping group, the MDL was 1.2±0.1µg/g, and higher mass collections did not improve upon this result. This MDL is comparable to chromium concentration levels seen in various studies involving human nail clippings. Further improvements to the portable XRF technique would be required to detect chromium levels expected from the lower end of a typical population.

  18. Semiconductor applications of nanoliter droplet methodology with total reflection x-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Miller, Thomasin C.; Sparks, Christopher M.; Havrilla, George J. E-mail: havrilla@lanl.gov; Beebe, Meredith R

    2004-08-31

    In this study, the nanoliter dried spot method was applied to semiconductor contamination analysis to enhance vapor phase decomposition processes with total reflection X-ray fluorescence detection. Nanoliter-sized droplets (10 and 50 nl) were deposited onto native silicon oxide wafer surfaces in a clean room environment from both single and multielemental standards containing various concentrations of iron in different matrices. Direct comparisons were made to droplets formed by conventional VPD with similar iron standards. Nanoliter dried spots could be reproducibly deposited and dried in air with typical drying times ranging from 20 s to 2 min depending on the nanoliter volume deposited, compared to VPD spots which have drying times ranging from tens of minutes to several hours. Both types of residues showed a linear relationship between Fe intensity and mass deposited. Variable angle experiments showed that both nanoliter and VPD deposits of single element standards were film-like in character, while residues formed from much more complex matrices and higher mass loadings were particulate in character. For the experimental conditions used in this study (30 kV, 100 mA), typical TXRF spectral Fe limits of detection were calculated to be on the order of picograms or {approx}1x10{sup 10} atoms/cm{sup 2} for a 0.8 cm{sup 2} X-ray excitation beam area for both nanoliter dried spots and VPD spots prepared from single elemental standards. Calculated Fe detection limits for 200 mm diameter silicon wafers used in this study were in the {approx}1x10{sup 8} atoms/cm{sup 2} range. By using nanoliter sized droplets, the required sample volume is greatly reduced resulting in higher sample throughput than with conventional VPD methods.

  19. Determination of trace element levels in leaves of Nerium oleander using X-Ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Ramon S.; Sanches, Francis A.C.R.A.; Neves, Arthur O.P.; Oliveira, Luis F.; Oliveira, Davi F.; Anjos, Marcelino J. [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Inst. de Fisica Armando Dias Tavares. Dept. de Fisica Aplicada e Termodinamica

    2013-07-01

    The environmental pollution by human activity has been one of the most concerns in the last years, principally due to rapid urban growth in the cities and the industrialization process. The air pollution can be increased due to several different kinds of emissions: urban traffic, industrial activities, burning fuel, civil industry of construction/demolition, fires and natural phenomena. Many of these emissions move from long distances due to convections currents and finally tend to deposit mainly in the plants leaves and in the soil. Thus, the plants leaves works as a natural sampler by the emissions deposit in these ones. In this study Nerium oleander leaves were used to measure the environmental pollutions levels in different sampling urban regions in the city of Rio de Janeiro/RJ: Andarai, Benfica, Bonsucesso, Caju, Engenho de Dentro, Engenho Novo, Estacio, Grajau, Inhauma, Lins, Maracana, Maria da Graca, Meier, Praca da Bandeira, Riachuelo, Rio Comprido, Sao Cristovao, Tijuca, Vila Isabel and city Center. The control samples were collected in Campo Grande near of Parque Nacional da Pedra Branca/RJ (National Park of Pedra Branca/RJ). The leaves were collected from adult plants and after the collection the samples were cleaned and placed in the greenhouse for drying, then were mashed and pressed into tablets forms. The analyses were performed using the energy dispersion X-ray fluorescence (EDXRF), developed on the own laboratory and based in a SiPIN detector and a mini X ray tube. It was possible to detect 16 elements in the analyzed samples: K, Ca, Cr, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba and Pb. The results shows that, in the studied areas, the analysis of the Nerium oleander plant shows a low-cost option and with a substantial efficiency as an environmental pollution biomonitor. (author)

  20. High energy x-ray diffraction/x-ray fluorescence spectroscopy for high-throughput analysis of composition spread thin films.

    Science.gov (United States)

    Gregoire, John M; Dale, Darren; Kazimirov, Alexander; DiSalvo, Francis J; van Dover, R Bruce

    2009-12-01

    High-throughput crystallography is an important tool in materials research, particularly for the rapid assessment of structure-property relationships. We present a technique for simultaneous acquisition of diffraction images and fluorescence spectra on a continuous composition spread thin film using a 60 keV x-ray source. Subsequent noninteractive data processing provides maps of the diffraction profiles, thin film fiber texture, and composition. Even for highly textured films, our diffraction technique provides detection of diffraction from each family of Bragg reflections, which affords direct comparison of the measured profiles with powder patterns of known phases. These techniques are important for high throughput combinatorial studies as they provide structure and composition maps which may be correlated with performance trends within an inorganic library.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sitko, Rafal, E-mail: rafal.sitko@us.edu.p [Institute of Chemistry, Silesian University, 40-006 Katowice (Poland)

    2009-11-15

    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

  2. On the emitting region of X-ray fluorescent lines around Compton-thick AGN

    CERN Document Server

    Liu, Jiren

    2016-01-01

    X-ray fluorescent lines are unique features of the reflection spectrum of the torus when irradiated by the central AGN. Their intrinsic line width can be used to probe the line-emitting region. Previous studies have focused on the Fe Ka line at 6.4 keV, which is the most prominent fluorescent line. These studies, however, are limited by the spectral resolution of currently available instruments, the best of which is $\\sim1860$ km s$^{-1}$ afforded by the Chandra High-Energy Grating (HEG). The HEG spectral resolution is improved by a factor of 4 at 1.74 keV, where the Si Ka line is located. We measured the FWHM of the Si Ka line for Circinus, Mrk 3, and NGC 1068, which are $570\\pm240$, $730\\pm320$, and $320\\pm280$ km s$^{-1}$, respectively. They are $3-5$ times smaller than those measured with the Fe Ka line previously. It shows that the intrinsic widths of the Fe Ka line are most likely to be over-estimated. The measured widths of the Si Ka line put the line-emitting region outside the dust sublimation radius...

  3. X-ray Fluorescence Tomography of Aged Fluid-Catalytic-Cracking Catalyst Particles Reveals Insight into Metal Deposition Processes

    NARCIS (Netherlands)

    Kalirai, Samanbir; Boesenberg, Ulrike; Falkenberg, Gerald; Meirer, Florian; Weckhuysen, Bert M.

    2015-01-01

    Microprobe X-ray fluorescence tomography was used to investigate metal poison deposition in individual, intact and industrially deactivated fluid catalytic cracking (FCC) particles at two differing catalytic life-stages. 3D multi-element imaging, at submicron resolution was achieved by using a large

  4. Analytical Instrument of X-ray Fluorescence Determine Concentration of U and Pu in Organic Solution at the Same Time

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    An instrument is developed to measure the concentration of U, Pu and the intensity of gamma ray in samples of 1AP organic phase at the same time. The Ag cold cathode is used to excite L series X-ray fluorescence of U and Pu. The Si-pin detector is

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-11-15

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

  6. X-ray fluorescence spectrometry applied to soil analysis; Espectrometria de fluorescencia de raios X aplicada as analises de solo

    Energy Technology Data Exchange (ETDEWEB)

    Salvador, Vera Lucia Ribeiro; Sato, Ivone Mulako; Scapin Junior, Wilson Santo; Scapin, Marcos Antonio; Imakima, Kengo [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil). E-mail: vsalvado@baitaca.ipen.br; imsato@net.ipen.br; kengo@sup.ipen.br

    1997-07-01

    This paper studies the X-ray fluorescence spectrometry applied to the soil analysis. A comparative study of the WD-XRFS and ED-XRFS techniques was carried out by using the following soil samples: SL-1, SOIL-7 and marine sediment SD-M-2/TM, from IAEA, and clay, JG-1a from Geological Survey of Japan (GSJ)

  7. X-ray Fluorescence Observations of the Moon by SMART-1/D-CIXS

    Science.gov (United States)

    Grande, Manuel; Swinyard, B.; Joy, K. H.; Kellett, Barry J.; Crawford, Ian A.; Howe, Chris J.

    2008-09-01

    Introduction The SMART-1 mission to the Moon included in its payload D-CIXS, a compact X-ray spectrometer [1], [2] SMART-1 was a technology evaluation mission, and D-CIXS was the first of a new generation of planetary X-ray spectrometers. Novel technologies enabled new capabilities for measuring the fluorescent yield of a planetary surface or atmosphere which is illuminated by solar X-rays. During the extended SMART-1 cruise phase, observations of the Earth showed strong argon emission, providing a good source for calibration and demonstrating the potential of the technique. At the Moon, observations showed a first unambiguous remote sensing of calcium in the lunar regolith (Grande et al 2007) (Fig 1). Data obtained were broadly consistent with current understanding of mare and highland composition. Ground truth was provided by the returned Apollo and Luna sample sets. We have extended our observations to comparisons of Lunar near and farside, and by careful analysis enabled new elemental lines to be observed. Observations: In March, 2005, the SMART-1 spacecraft reached its nominal lunar orbit, and we began full commissioning for lunar operations. During the pre-commissioning period in mid-January, 2005, observations of the lunar surface were made which coincided with the occurrence of several major M and X class flares. This opportunity provided an excellent chance to observe spatially localized fluorescence from the lunar surface. X-ray fluorescent elemental lines from the lunar surface are detected by all three facets of D-CIXS while the XSM instrument observes the input solar spectrum. At the end of this interval, a long duration M-class solar flare began at 06:00 UTC on the 15th of January, 2005. The flare lasted for more than 1 hour but only ~30 minutes corresponded to D-CIXS observations. At this time SMART-1 was orbiting over the Moon's near-side eastern limb from about the equator, traveling northwards. As SMART-1 flew north, its altitude was also

  8. X-ray fluorescence for quantification of lead and strontium in vivo

    Science.gov (United States)

    Specht, Aaron James

    Lead (Pb) is a toxicant well known for its effects on almost every organ system in the body. Pb use in industry has declined since removal of Pb from gasoline, but many developing countries still have significant use of Pb. Exposure to Pb has been linked with diseases causing neurodegeneration and thus have lasting effects long after the initial exposure. Another metal, strontium (Sr), has been linked with bone disease in particular situations and shown to have uses in treating osteoporosis as a supplement. However, there are no studies of the effects of Sr using a meaningful biomarker. The most commonly used biomarkers for Pb and Sr exposures are blood Pb and Sr; however, blood tests are unable to identify long-term exposure levels due to the short half-life of these metals in blood. Bone stores of Pb and Sr have a half-life of years to decades and serve as a biomarker of long-term exposure. X-ray fluorescence has been used to measure bone Pb and Sr. However, current systems have limitations with radioisotope sources, bulky equipment, and long measurement times. A portable XRF device capable of measurement of bone Pb and Sr, overcomes the limitation of the current systems and has been developed in this work. The detection limit of the portable XRF for bone Pb and Sr was found to be 11 ppm and 5 ppm respectively at 5 mm of skin thickness. The portable XRF will have limitations of measurement based on an individual's skin thickness. The device was calibrated using standard phantoms and validated with in-lab samples, which demonstrated good agreement between KXRF and portable XRF measurements with strong correlations between goat bone, cadaver bone, and phantom measurements. In a population study of Pb poisoned children the portable XRF was further validated and a significant correlation between KXRF measured bone Pb and portable XRF measured bone Pb was identified; however, the device had limitations based on anatomical differences unaccounted for in children from

  9. Probing the graphite band structure with resonant soft-x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Carlisle, J.A.; Shirley, E.L.; Hudson, E.A. [Lawrence Berkeley National Lab., CA (United States)] [and others

    1997-04-01

    Soft x-ray fluorescence (SXF) spectroscopy using synchrotron radiation offers several advantages over surface sensitive spectroscopies for probing the electronic structure of complex multi-elemental materials. Due to the long mean free path of photons in solids ({approximately}1000 {angstrom}), SXF is a bulk-sensitive probe. Also, since core levels are involved in absorption and emission, SXF is both element- and angular-momentum-selective. SXF measures the local partial density of states (DOS) projected onto each constituent element of the material. The chief limitation of SXF has been the low fluorescence yield for photon emission, particularly for light elements. However, third generation light sources, such as the Advanced Light Source (ALS), offer the high brightness that makes high-resolution SXF experiments practical. In the following the authors utilize this high brightness to demonstrate the capability of SXF to probe the band structure of a polycrystalline sample. In SXF, a valence emission spectrum results from transitions from valence band states to the core hole produced by the incident photons. In the non-resonant energy regime, the excitation energy is far above the core binding energy, and the absorption and emission events are uncoupled. The fluorescence spectrum resembles emission spectra acquired using energetic electrons, and is insensitive to the incident photon`s energy. In the resonant excitation energy regime, core electrons are excited by photons to unoccupied states just above the Fermi level (EF). The absorption and emission events are coupled, and this coupling manifests itself in several ways, depending in part on the localization of the empty electronic states in the material. Here the authors report spectral measurements from highly oriented pyrolytic graphite.

  10. Total reflection X-ray fluorescence trace mercury determination by trapping complexation: Application in advanced oxidation technologies

    Energy Technology Data Exchange (ETDEWEB)

    Custo, Graciela [Unidad de Actividad Quimica, Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina); Litter, Marta I. [Unidad de Actividad Quimica, Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina); Escuela de Posgrado, Universidad de General San Martin, San Lorenzo 3391 Villa Ballester, 1653. Prov. de Buenos Aires (Argentina); Rodriguez, Diana [Universidad Nacional de Lujan, Ruta 5 y 7. Prov. de Buenos Aires (Argentina); Vazquez, Cristina [Unidad de Actividad Quimica, Comision Nacional de Energia Atomica, Av. Gral Paz 1499 (B1650KNA) San Martin, Buenos Aires (Argentina) and 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

    2006-11-15

    It is well known that Hg species cause high noxious effects on the health of living organisms even at very low levels (5 {mu}g/L). Quantification of this element is an analytical challenge due to the peculiar physicochemical properties of all Hg species. The regulation of the maximal allowable Hg concentration led to search for sensitive methods for its determination. Total reflection X-ray fluorescence is a proved instrumental analytical tool for the determination of trace elements. In this work, the use of total reflection X-ray fluorescence for Hg quantification is investigated. However, experimental determination by total reflection X-ray fluorescence requires depositing a small volume of sample on the reflector and evaporation of the solvent until dryness to form a thin film. Because of volatilization of several Hg forms, a procedure to capture these volatile species in liquid samples by using complexing agents is proposed. Acetate, oxalic acid, ethylenediaminetetracetic acid and ammonium pyrrolidine-dithiocarbamate were assayed for trapping the analytes into the solution during the preparation of the sample and onto the reflector during total reflection X-ray fluorescence measurements. The proposed method was applied to evaluate Hg concentration during TiO{sub 2}-heterogeneous photocatalysis, one of the most known advanced oxidation technologies. Advanced oxidation technologies are processes for the treatment of effluents in waters and air that involve the generation of very active oxidative and reductive species. In heterogeneous photocatalysis, Hg is transformed to several species under ultraviolet illumination in the presence of titanium dioxide. Total reflection X-ray fluorescence was demonstrated to be applicable in following the extent of the heterogeneous photocatalysis reaction by determining non-transformed Hg in the remaining solution.

  11. Total reflection X-ray fluorescence trace mercury determination by trapping complexation: Application in advanced oxidation technologies

    Science.gov (United States)

    Custo, Graciela; Litter, Marta I.; Rodríguez, Diana; Vázquez, Cristina

    2006-11-01

    It is well known that Hg species cause high noxious effects on the health of living organisms even at very low levels (5 μg/L). Quantification of this element is an analytical challenge due to the peculiar physicochemical properties of all Hg species. The regulation of the maximal allowable Hg concentration led to search for sensitive methods for its determination. Total reflection X-ray fluorescence is a proved instrumental analytical tool for the determination of trace elements. In this work, the use of total reflection X-ray fluorescence for Hg quantification is investigated. However, experimental determination by total reflection X-ray fluorescence requires depositing a small volume of sample on the reflector and evaporation of the solvent until dryness to form a thin film. Because of volatilization of several Hg forms, a procedure to capture these volatile species in liquid samples by using complexing agents is proposed. Acetate, oxalic acid, ethylenediaminetetracetic acid and ammonium pyrrolidine-dithiocarbamate were assayed for trapping the analytes into the solution during the preparation of the sample and onto the reflector during total reflection X-ray fluorescence measurements. The proposed method was applied to evaluate Hg concentration during TiO 2-heterogeneous photocatalysis, one of the most known advanced oxidation technologies. Advanced oxidation technologies are processes for the treatment of effluents in waters and air that involve the generation of very active oxidative and reductive species. In heterogeneous photocatalysis, Hg is transformed to several species under ultraviolet illumination in the presence of titanium dioxide. Total reflection X-ray fluorescence was demonstrated to be applicable in following the extent of the heterogeneous photocatalysis reaction by determining non-transformed Hg in the remaining solution.

  12. A study of ancient pottery by means of X-ray fluorescence spectroscopy, multivariate statistics and mineralogical analysis

    Energy Technology Data Exchange (ETDEWEB)

    Papachristodoulou, Christina [Nuclear Physics Laboratory, Department of Physics, University of Ioannina, 451 10 Ioannina (Greece); Oikonomou, Artemios [Composite Materials Laboratory, Department of Materials' Science and Engineering, University of Ioannina, 451 10 Ioannina (Greece); Ioannides, Kostas [Nuclear Physics Laboratory, Department of Physics, University of Ioannina, 451 10 Ioannina (Greece); Gravani, Konstantina [Archaelogy Section, Department of History-Archaeology, University of Ioannina, 451 10 Ioannina (Greece)

    2006-07-28

    Energy-dispersive X-ray fluorescence spectroscopy was used to determine the composition of 64 potsherds from the Hellenistic settlement of Orraon, in northwestern Greece. Data classification by principal components analysis revealed four distinct groups of pottery, pointing to different local production practices rather than different provenance. The interpretation of statistical grouping was corroborated by a complementary X-ray diffraction analysis. Compositional and mineralogical data, combined with archaeological and materials' science criteria, allowed addressing various aspects of pottery making, such as selection of raw clays, tempers and firing conditions.

  13. A study of ancient pottery by means of X-ray fluorescence spectroscopy, multivariate statistics and mineralogical analysis.

    Science.gov (United States)

    Papachristodoulou, Christina; Oikonomou, Artemios; Ioannides, Kostas; Gravani, Konstantina

    2006-07-28

    Energy-dispersive X-ray fluorescence spectroscopy was used to determine the composition of 64 potsherds from the Hellenistic settlement of Orraon, in northwestern Greece. Data classification by principal components analysis revealed four distinct groups of pottery, pointing to different local production practices rather than different provenance. The interpretation of statistical grouping was corroborated by a complementary X-ray diffraction analysis. Compositional and mineralogical data, combined with archaeological and materials' science criteria, allowed addressing various aspects of pottery making, such as selection of raw clays, tempers and firing conditions.

  14. X-ray fluorescence activities at Saha Institute of Nuclear Physics, India

    Indian Academy of Sciences (India)

    Manoranjan Sarkar

    2011-02-01

    This paper covers different aspects related to X-ray fluorescence activities at Saha Institute of Nuclear Physics, Kolkata, India. In its first part, experiments on basic physical problems are illustrated and in the second part, some applications related to X-ray fluorescence are discussed.

  15. Bibliography of NRL Works on X-Ray Fluorescence Authored by L. S. Birks, D. B. Brown, J. W. Criss, H. Friedman, and J. V. Gilfrich

    Science.gov (United States)

    2007-11-02

    1720-1725 (1987). 340 C. M. Dozier, D. M. Fleetwood, D. B. Brown et al., "An Evaluation of Low-Energy X-Ray and Cobalt -60 Irradiations of Mos-Transistors...P. S. Winokur, C. M. Dozier et al., "Effect of Bias on the Response of Metal-Oxide- Semiconductor Devices to Low-Energy X-Ray and Cobalt -60...analysis at the ICDD ," X-Ray Spectrometry 26 (5), 247 (1997). 438 J. Gilfrich, "Micro x-ray fluorescence analysis," X-Ray Spectrometry 26 (3), 95 (1997

  16. Investigation of measuring hazardous substances in printed circuit boards using the micro-focus X-ray fluorescence screening

    CERN Document Server

    Fu, M L; Fakhrtdinov, R; Grigoriev, M; Quan, B S; Le, Z C; Roshchupkin, D

    2014-01-01

    Printed circuit boards (PCBs) are widely used in most electrical and electronic equipments or products. Hazardous substances such as Pb, Hg, Cd, etc, can be present in high concentrations in PCBs and the degradation and release of these substances poses a huge threat to humans and the environment. To investigation the chemical composition of PCBs in domestic market of China, a practical micro-focus X-ray fluorescence system is setup to make the elements analysis, especially for detecting hazardous substances. Collimator is adopted to focus the X-ray emitted from X-ray tube. BRUKER X-ray detector with proportional counter is used to detect the emitted fluorescence from the PCB samples. Both single layer PCB samples and double layers PCB samples made of epoxy glass fiber are purchased from the domestic market of China. Besides, a MC55 wireless communication module made by SIEMENS in Germany is used as the reference material. Experimental results from the fluorescence spectrums of the testing points of PCB sampl...

  17. Characterisation of mineralisation of bone and cartilage: X-ray diffraction and Ca and Sr K α X-ray fluorescence microscopy

    Science.gov (United States)

    Bradley, D. A.; Muthuvelu, P.; Ellis, R. E.; Green, E. M.; Attenburrow, D.; Barrett, R.; Arkill, K.; Colridge, D. B.; Winlove, C. P.

    2007-10-01

    Bone is a dynamic structure, constantly remodelling in response to changing mechanical and environmental factors. This is particularly evident in the mineral component encrusting the collagenous framework. The mineral is principally in the form of calcium apatite, but calcium can exchange with strontium, both during the cellular processes of mineralisation and resorption and by passive exchange with the deposited crystals. Mineralisation is generally characterized by densitometry, but because of the differences in absorption cross sections of calcium and strontium it can be misleading in studies of composition. In this work we have used X-ray diffraction to identify calcium and strontium apatite and X-ray fluorescence to quantify strontium and calcium distribution. With the beam characteristics available from synchrotron radiation, this has enabled us to obtain microscopic resolution on thin sections of bone and cartilage from the equine metacarpophalangeal joint. Two issues have been investigated; the first is the distribution of mineral in the bone-cartilage interface and within individual trabeculae. In trabecular bone the ratio of strontium to calcium concentration was typically 0.0035 ± 0.0020, and higher by a factor of ∼3 at the periphery than in the centre of a trabeculum (possibly reflecting the more rapid turnover of mineral in the surface layer). In the dense subchondral bone the ratio was similar, approximately doubling in the calcified cartilage. The second objective was to explore the changes in mineralisation associated with development of osteoarthrosis. We analysed lesions showing cartilage thinning and changes in the trabecular organization and density of the underlying bone. At the centre of the lesion the ratio of strontium to calcium was much lower than that in normal tissue, although the calcified cartilage still showed a higher ratio than the underlying bone. In the superficially normal tissue around the lesion the calcified cartilage

  18. Characterisation of mineralisation of bone and cartilage: X-ray diffraction and Ca and Sr K{sub {alpha}} X-ray fluorescence microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bradley, D.A. [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford, Surrey, GU2 7XH (United Kingdom)], E-mail: d.a.bradley@surrey.ac.uk; Muthuvelu, P.; Ellis, R.E.; Green, E.M.; Attenburrow, D. [Biomedical Physics Group, School of Physics, University of Exeter, Exeter (United Kingdom); Barrett, R. [ESRF, BP 220, F-38043 Grenoble Cedex (France); Arkill, K.; Colridge, D.B.; Winlove, C.P. [Biomedical Physics Group, School of Physics, University of Exeter, Exeter (United Kingdom)

    2007-10-15

    Bone is a dynamic structure, constantly remodelling in response to changing mechanical and environmental factors. This is particularly evident in the mineral component encrusting the collagenous framework. The mineral is principally in the form of calcium apatite, but calcium can exchange with strontium, both during the cellular processes of mineralisation and resorption and by passive exchange with the deposited crystals. Mineralisation is generally characterized by densitometry, but because of the differences in absorption cross sections of calcium and strontium it can be misleading in studies of composition. In this work we have used X-ray diffraction to identify calcium and strontium apatite and X-ray fluorescence to quantify strontium and calcium distribution. With the beam characteristics available from synchrotron radiation, this has enabled us to obtain microscopic resolution on thin sections of bone and cartilage from the equine metacarpophalangeal joint. Two issues have been investigated; the first is the distribution of mineral in the bone-cartilage interface and within individual trabeculae. In trabecular bone the ratio of strontium to calcium concentration was typically 0.0035 {+-} 0.0020, and higher by a factor of {approx}3 at the periphery than in the centre of a trabeculum (possibly reflecting the more rapid turnover of mineral in the surface layer). In the dense subchondral bone the ratio was similar, approximately doubling in the calcified cartilage. The second objective was to explore the changes in mineralisation associated with development of osteoarthrosis. We analysed lesions showing cartilage thinning and changes in the trabecular organization and density of the underlying bone. At the centre of the lesion the ratio of strontium to calcium was much lower than that in normal tissue, although the calcified cartilage still showed a higher ratio than the underlying bone. In the superficially normal tissue around the lesion the calcified

  19. Coelectrodeposition of Ternary Mn-Oxide/Polypyrrole Composites for ORR Electrocatalysts: A Study Based on Micro-X-ray Absorption Spectroscopy and X-ray Fluorescence Mapping

    Directory of Open Access Journals (Sweden)

    Benedetto Bozzini

    2015-08-01

    Full Text Available Low energy X-ray fluorescence (XRF and soft X-ray absorption (XAS microspectroscopies at high space-resolution are employed for the investigation of the coelectrodeposition of composites consisting of a polypyrrole(PPy-matrix and Mn-based ternary dispersoids, that have been proposed as promising electrocatalysts for oxygen-reduction electrodes. Specifically, we studied Mn–Co–Cu/PP, Mn–Co–Mg/PPy and Mn–Ni–Mg/PPy co-electrodeposits. The Mn–Co–Cu system features the best ORR electrocatalytic activity in terms of electron transfer number, onset potential, half-wave potential and current density. XRF maps and micro-XAS spectra yield compositional and chemical state distributions, contributing unique molecular-level information on the pulse-plating processes. Mn, Ni, Co and Mg exhibit a bimodal distribution consisting of mesoscopic aggregates of micrometric globuli, separated by polymer-rich ridges. Within this common qualitative scenario, the individual systems exhibit quantitatively different chemical distribution patterns, resulting from specific electrokinetic and electrosorption properties of the single components. The electrodeposits consist of Mn3+,4+-oxide particles, accompanied by combinations of Co0/Co2+, Ni0/Ni2+ and Cu0,+/Cu2+ resulting from the alternance of cathodic and anodic pulses. The formation of highly electroactive Mn3+,4+ in the as-fabricated material is a specific feature of the ternary systems, deriving from synergistic stabilisation brought about by two types of bivalent dopants as well as by galvanic contact to elemental metal; this result represents a considerable improvement in material quality with respect to previously studied Mn/PPy and Mn-based/PPy binaries.

  20. Determination of element levels in human serum: Total reflection X-ray fluorescence applications

    Science.gov (United States)

    Majewska, U.; Łyżwa, P.; Łyżwa, K.; Banaś, D.; Kubala-Kukuś, A.; Wudarczyk-Moćko, J.; Stabrawa, I.; Braziewicz, J.; Pajek, M.; Antczak, G.; Borkowska, B.; Góźdź, S.

    2016-08-01

    Deficiency or excess of elements could disrupt proper functioning of the human body and could lead to several disorders. Determination of their concentrations in different biological human fluids and tissues should become a routine practice in medical treatment. Therefore the knowledge about appropriate element concentrations in human organism is required. The purpose of this study was to determine the concentration of several elements (P, S, Cl, K, Ca, Cr, Fe, Cu, Zn, Se, Br, Rb, Pb) in human serum and to define the reference values of element concentration. Samples of serum were obtained from 105 normal presumably healthy volunteers (66 women aged between 15 and 78 years old; 39 men aged between 15 and 77 years old). Analysis has been done for the whole studied population and for subgroups by sex and age. It is probably first so a wide study of elemental composition of serum performed in the case of Świętokrzyskie region. Total reflection X-ray fluorescence (TXRF) method was used to perform the elemental analysis. Spectrometer S2 Picofox (Bruker AXS Microanalysis GmbH) was used to identify and measure elemental composition of serum samples. Finally, 1st and 3rd quartiles were accepted as minimum and maximum values of concentration reference range.

  1. Sample sizing of biological materials analyzed by energy dispersion X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Paiva, Jose D.S.; Franca, Elvis J.; Magalhaes, Marcelo R.L.; Almeida, Marcio E.S.; Hazin, Clovis A., E-mail: dan-paiva@hotmail.com, E-mail: ejfranca@cnen.gov.br, E-mail: marcelo_rlm@hotmail.com, E-mail: maensoal@yahoo.com.br, E-mail: chazin@cnen.gov.b [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

    2013-07-01

    Analytical portions used in chemical analyses are usually less than 1g. Errors resulting from the sampling are barely evaluated, since this type of study is a time-consuming procedure, with high costs for the chemical analysis of large number of samples. The energy dispersion X-ray fluorescence - EDXRF is a non-destructive and fast analytical technique with the possibility of determining several chemical elements. Therefore, the aim of this study was to provide information on the minimum analytical portion for quantification of chemical elements in biological matrices using EDXRF. Three species were sampled in mangroves from the Pernambuco, Brazil. Tree leaves were washed with distilled water, oven-dried at 60 deg C and milled until 0.5 mm particle size. Ten test-portions of approximately 500 mg for each species were transferred to vials sealed with polypropylene film. The quality of the analytical procedure was evaluated from the reference materials IAEA V10 Hay Powder, SRM 2976 Apple Leaves. After energy calibration, all samples were analyzed under vacuum for 100 seconds for each group of chemical elements. The voltage used was 15 kV and 50 kV for chemical elements of atomic number lower than 22 and the others, respectively. For the best analytical conditions, EDXRF was capable of estimating the sample size uncertainty for further determination of chemical elements in leaves. (author)

  2. Quantitative Imaging of Cell-Permeable Magnetic Resonance Contrast Agents Using X-Ray Fluorescence

    Directory of Open Access Journals (Sweden)

    Paul J. Endres

    2006-10-01

    Full Text Available The inability to transduce cellular membranes is a limitation of current magnetic resonance imaging probes used in biologic and clinical settings. This constraint confines contrast agents to extracellular and vascular regions of the body, drastically reducing their viability for investigating processes and cycles in developmental biology. Conversely, a contrast agent with the ability to permeate cell membranes could be used in visualizing cell patterning, cell fate mapping, gene therapy, and, eventually, noninvasive cancer diagnosis. Therefore, we describe the synthesis and quantitative imaging of four contrast agents with the capability to cross cell membranes in sufficient quantity for detection. Each agent is based on the conjugation of a Gd(III chelator with a cellular transduction moiety. Specifically, we coupled Gd(III–diethylenetriaminepentaacetic acid DTPA and Gd(III–1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid with an 8–amino acid polyarginine oligomer and an amphipathic stilbene molecule, 4-amino-4'-(N,N-dimethylaminostilbene. The imaging modality that provided the best sensitivity and spatial resolution for direct detection of the contrast agents is synchrotron radiation x-ray fluorescence (SR-XRF. Unlike optical microscopy, SR-XRF provides two-dimensional images with resolution 103 better than 153Gd gamma counting, without altering the agent by organic fluorophore conjugation. The transduction efficiency of the intracellular agents was evaluated by T1 analysis and inductively coupled plasma mass spectrometry to determine the efficacy of each chelate-transporter combination.

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

    Science.gov (United States)

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

    2015-11-01

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

  4. Total reflection X-ray fluorescence as a fast multielemental technique for human placenta sample analysis

    Science.gov (United States)

    Marguí, E.; Ricketts, P.; Fletcher, H.; Karydas, A. G.; Migliori, A.; Leani, J. J.; Hidalgo, M.; Queralt, I.; Voutchkov, M.

    2017-04-01

    In the present contribution, benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been evaluated as a cost-effective multielemental analytical technique for human placenta analysis. An easy and rapid sample preparation consisting of suspending 50 mg of sample in 1 mL of a Triton 1% solution in deionized water showed to be the most suitable for this kind of samples. However, for comparison purposes, an acidic microwave acidic digestion procedure was also applied. For both sample treatment methodologies, limits of detection for most elements were in the low mg/kg level. Accurate and precise results were obtained using internal standardization as quantification approach and applying a correction factor to compensate for absorption effects. The correction factor was based on the proportional ratio between the slurry preparation results and those obtained for the analysis of a set of human placenta samples analysed by microwave acidic digestion and ICP-AES analysis. As a study case, the developed TXRF methodology was applied for multielemental analysis (K, Ca, Fe, Cu, Zn, As, Se, Br, Rb and Sr) of several healthy women's placenta samples from two regions in Jamaica.

  5. Study of the hydrogen peroxide bleaching agent effects on bovine enamel using X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Ruda F.; Calazans, Fernanda S.; Miranda, Mauro S.; Santos, Ramon S.; Anjos, Marcelino J.; Assis, Joaquim T. [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil)

    2013-07-01

    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)

  6. Non-destructive investigation of a time capsule using neutron radiography and X-ray fluorescence

    Science.gov (United States)

    MacDonald, B. L.; Vanderstelt, J.; O'Meara, J.; McNeill, F. E.

    2016-01-01

    Non-destructive analytical techniques are becoming increasingly important for the study of objects of cultural heritage interest. This study applied two techniques: X-ray fluorescence and neutron radiography, for the investigation of a capped, tubular metal object recovered from an urban construction site in Gore Park, Hamilton, Canada. The site is an urban park containing a World War I commemorative monument that underwent renovation and relocation. Historical documentation suggested that the object buried underneath the monument was a time capsule containing a paper document listing the names of 1800 Canadians who died during WWI. The purpose of this study was to assess the condition of the object, and to verify if it was what the historical records purported. XRF analysis was used to characterize the elemental composition of the metal artifact, while neutron radiography revealed that its contents were congruent with historical records and remained intact after being interred for 91 years. Results of this study demonstrate the value of non-destructive techniques for the analysis and preservation of cultural heritage.

  7. Iontophoresis: mechanism of action studied by potentiometry and x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Puttemans, F.J.; Massart, D.L.; Gilles, F.; Lievens, P.C.; Jonckeer, M.H.

    1982-04-01

    Physiotherapists often apply electrotherapeutic treatments to the knees with sponges impregnated with potassium iodide (KI). To study the fate of iodine applied in this way, the amount of iodide (I-) that penetrates the skin was determined using an iodide-selective electrode. The I- uptake was shown to take place only when galvanic current was applied. Iontophoresis did not result in superficial migration of the applied ions on the skin from one pole to the other, but led to penetration into the skin. The hyperemia, which occurs at the zone of application during iontophoresis, did not affect the uptake of subsequent treatments. Only very slight differences in uptake were observed for each patient with sequential application, whereas the interindividual differences were more pronounced. Combined evidence from all experiments suggested that about 10% of the applied KI had penetrated the skin. X-ray fluorescence scans of the volunteers' thyroid gland, before and after a series of 10 iontophoretic treatments, to establish whether I- was taken up by the thyroid, showed that the average iodine content of the gland was increased by more than 30%.

  8. High temperature monitoring of silicon carbide ceramics by confocal energy dispersive X-ray fluorescence spectrometry

    Science.gov (United States)

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi

    2016-04-01

    In the present work, we presented an alternative method for monitoring of the oxidation situation of silicon carbide (SiC) ceramics at various high temperatures in air by measuring the Compton-to-Rayleigh intensity ratios (ICo/IRa) and effective atomic numbers (Zeff) of SiC ceramics with the confocal energy dispersive X-ray fluorescence (EDXRF) spectrometer. A calibration curve of the relationship between ICo/IRa and Zeff was established by using a set of 8 SiC calibration samples. The sensitivity of this approach is so high that it can be easily distinguished samples of Zeff differing from each other by only 0.01. The linear relationship between the variation of Zeff and the variations of contents of C, Si and O of SiC ceramics were found, and the corresponding calculation model of the relationship between the ΔZ and the ΔCC, ΔCSi, and ΔCO were established. The variation of contents of components of the tested SiC ceramics after oxidation at high temperature was quantitatively calculated based on the model. It was shown that the results of contents of carbon, silicon and oxygen obtained by this method were in good agreement with the results obtained by XPS, giving values of relative deviation less than 1%. It was concluded that the practicality of this proposed method for monitoring of the oxidation situation of SiC ceramics at high temperatures was acceptable.

  9. Non-destructive investigation of a time capsule using neutron radiography and X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    MacDonald, B.L., E-mail: macdonbl@mcmaster.ca [McMaster University, Department of Medical Physics and Applied Radiation Sciences, Hamilton (Canada); Vanderstelt, J., E-mail: joshv@nray.ca [Nray Services Inc., 56A Head Street, Dundas, ON (Canada); O’Meara, J. [University of Guelph, Department of Physics, Guelph (Canada); McNeill, F.E. [McMaster University, Department of Medical Physics and Applied Radiation Sciences, Hamilton (Canada)

    2016-01-15

    Non-destructive analytical techniques are becoming increasingly important for the study of objects of cultural heritage interest. This study applied two techniques: X-ray fluorescence and neutron radiography, for the investigation of a capped, tubular metal object recovered from an urban construction site in Gore Park, Hamilton, Canada. The site is an urban park containing a World War I commemorative monument that underwent renovation and relocation. Historical documentation suggested that the object buried underneath the monument was a time capsule containing a paper document listing the names of 1800 Canadians who died during WWI. The purpose of this study was to assess the condition of the object, and to verify if it was what the historical records purported. XRF analysis was used to characterize the elemental composition of the metal artifact, while neutron radiography revealed that its contents were congruent with historical records and remained intact after being interred for 91 years. Results of this study demonstrate the value of non-destructive techniques for the analysis and preservation of cultural heritage.

  10. Determination of Ca/P molar ratio in hydroxyapatite (HA) by X-ray fluorescence technique

    Energy Technology Data Exchange (ETDEWEB)

    Scapin, Marcos A.; Guilhen, Sabine N.; Cotrim, Marycel E.B.; Pires, Maria Ap. F., E-mail: mascapin@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    Hydroxyapatite (HA) is a mineral composed of calcium phosphate employed for endodontics, restorative dentistry and other applications in orthopedics and prosthesis. Additionally, this biomaterial is an inexpensive but efficient adsorbent for the removal of heavy metals and other unwanted species of contaminated liquid effluents. This is especially interesting when low-cost effective remediation is required. A Ca / P molar ratio of 1.667 is consistent with the theoretical Ca / P ratio for calcium hydroxyapatite with a compositional formula of Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, which properties are well discussed in the literature. The aim of this work was to implement and validate a methodology for simultaneous determination of major and minor constituents in the hydroxyapatite (HA) as well as providing the Ca / P molar ratio. To accomplish these achievements, wavelength dispersive X-ray fluorescence spectroscopy (WDXRF) was applied. This is a non-destructive technique that requires no chemical treatment, enabling fast chemical analysis in a wide variety of samples, with no hazardous waste being generated as a result of the process of determination. A standard reference material from NIST (SRM 1400 – Bone Ash) was used to validate the methodology for the determination of magnesium, phosphorus, potassium, calcium, iron, zinc, strontium and the Ca / P ratio in HA samples by WDXRF. The Z-score test was applied as a statistical tool and showed that the calculated values were of less than 1.8 for all the measured analytes. (author)

  11. HIGH RESOLUTION X-RAY FLUORESCENCE MICRO-TOMOGRAPHY ON SINGLE SEDIMENT PARTICLES.

    Energy Technology Data Exchange (ETDEWEB)

    VINCZE,L.; VEKEMANS,B.; SZALOKI,I.; JANSSENS,K.; VAN GRIEKEN,R.; FENG,H.; JONES,K.W.; ADAMS,F.

    2002-07-29

    This work focuses on the investigation of the distribution of contaminants in individual sediment particles from the New York/New Jersey Harbor. Knowledge of the spatial distribution of the contaminants within the particles is needed to enable (1) more sophisticated approaches to the understanding of the fate and transport of the contaminants in the environment and (2) more refined methods for cleaning the sediments. The size of the investigated particles ranges from 30-80 microns. Due to the low concentration of the elements of interest and the microscopic size of the environmental particles in these measurements, the small size and high intensity of the analyzing X-ray beam was critical. The high photon flux at the ESRF Microfocus beam line (ID13) was used as the basis for fluorescence tomography to investigate whether the inorganic compounds are taken upon the surface organic coating or whether they are distributed through the volume of the grains being analyzed. The experiments were done using a 13 keV monochromatic beam of approximately 2 {micro}m in size having an intensity of 10{sup 10} ph/s, allowing absolute detection limits on the 0.04-1 fg level for Ti, Cr, Mn, Fe, Ni, and Zn.

  12. Determination of bromine in regulated foods with a field-portable X-ray fluorescence analyzer.

    Science.gov (United States)

    Anderson, David L

    2009-01-01

    A field-portable X-ray fluorescence analyzer, factory-calibrated for soil analysis, was used to measure bromine (Br) mass fractions in reference materials, flour, bakery products, malted barley, selected U.S. Food and Drug Administration Total Diet Study foods, and other food products. By using a calibration based on instrumental neutron activation analysis results for Br in reference materials, accurate quantitative results, confirmed by z-scores, could be obtained for mass fractions of about 2-55 mg/kg. These results confirmed accuracy of results (with larger uncertainties) obtained by applying a simple correction factor to the analyzer's output value. Results showed that very short analysis times (content at regulatory levels for brominated and enriched brominated flour (24 mg/kg Br) and whole wheat flour and bakery products (36 mg/kg Br). Feasibility for determination of Br in malted barley at the regulatory level (75 mg/kg Br) was demonstrated, but quantitative results at that level could not be assured because no reference material with a suitable mass fraction was available. Br mass fractions for all foods tested were well below regulatory levels.

  13. Comparison of gold leaf thickness in Namban folding screens using X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Pessanha, Sofia; Madeira, Teresa I.; Manso, Marta [Centro de Fisica Atomica da Universidade de Lisboa, Lisbon (Portugal); Guerra, Mauro; Carvalho, Maria Luisa [Centro de Fisica Atomica da Universidade de Lisboa, Lisbon (Portugal); Universidade Nova de Lisboa, Departamento de Fisica, Faculdade de Ciencias e Tecnologia, Caparica (Portugal); Gac, Agnes le [Centro de Fisica Atomica da Universidade de Lisboa, Lisbon (Portugal); Universidade Nova de Lisboa, Departamento de Conservacao e Restauro, Faculdade de Ciencias e Tecnologia, Caparica (Portugal)

    2014-09-15

    In this work, the thickness of the gold leaf applied in six Japanese folding screens is compared using a nondestructive approach. Four screens belonging to the Momoyama period (∝1573-1603) and two screens belonging to the early Edo period (∝1603-1868) were analyzed in situ using energy dispersive X-ray fluorescence, and the thickness of the applied gold leaf was evaluated using a methodology based on the attenuation of the different characteristic lines of gold in the gold leaf layer. Considering that the leaf may well not be made of pure gold, we established that, for the purpose of comparing the intensity ratios of the Au lines, layers made with gold leaf of high grade can be considered identical. The gold leaf applied in one of the screens from the Edo period was found to be thinner than the gold leaf applied in the other ones. This is consistent with the development of the beating technology to obtain ever more thin gold leafs. (orig.)

  14. Synchrotron radiation X-ray fluorescence analysis on altered mineral muscovite in gold deposit

    Institute of Scientific and Technical Information of China (English)

    TANG Yun-Hui; YUAN Wan-Ming; WANG Li-Hua; HAN Chun-Ming; HUANG Yu-Ying; HE Wei

    2005-01-01

    Synchrotron radiation X-ray fluorescence (SRXRF) microprobe was used to ananlyse altered mineral muscovite and its surrounding feldspar in Yuerya gold deposit. The major, minor and trace elements of the two minerals were detected and analyzed. SRXRF analysis showed that the Yuerya muscovite had a complex chemical composition, containing K, Fe, Ca, Ti, Cr, Mn, Co, Cu, Zn and many trace or ultra-trace elements. Since muscovite resulted from the alteration of hydrothermal ore fluid acting on feldspar (plagioclase), the difference of chemical composition between the two minerals shows the components of ore fluid, which are characterized by the enrichment of alkaline and alkaline-earth metal elements K, Ca and ore-associated elements Fe, Cu, Zn. And gold, silver and platinum, invisible under microscope, were detected in some areas of muscovite, but not found in feldspar. Especially platinum, a mantle material, is rarely seen in the earth crust but now found in the gold deposit of magmatic sources; its appearance approves the idea of mantle flux participating in the gold mineralization, which suggests that the tectonic event controlling gold mineralization in the Yuerya district is a mantle phenomenon.

  15. Synchrotron X-ray fluorescence spectroscopy of salts in natural sea ice

    Science.gov (United States)

    Obbard, Rachel W.; Lieb-Lappen, Ross M.; Nordick, Katherine V.; Golden, Ellyn J.; Leonard, Jeremiah R.; Lanzirotti, Antonio; Newville, Mathew G.

    2016-11-01

    We describe the use of synchrotron-based X-ray fluorescence spectroscopy to examine the microstructural location of specific elements, primarily salts, in sea ice. This work was part of an investigation of the location of bromine in the sea ice-snowpack-blowing snow system, where it plays a part in the heterogeneous chemistry that contributes to tropospheric ozone depletion episodes. We analyzed samples at beamline 13-ID-E of the Advanced Photon Source at Argonne National Laboratory. Using an 18 keV incident energy beam, we produced elemental maps of salts for sea ice samples from the Ross Sea, Antarctica. The distribution of salts in sea ice depends on ice type. In our columnar ice samples, Br was located in parallel lines spaced roughly 0.5 mm apart, corresponding to the spacing of lamellae in the skeletal region during initial ice growth. The maps revealed concentrations of Br in linear features in samples from all but the topmost and bottommost depths. For those samples, the maps revealed rounded features. Calibration of the Br elemental maps showed bulk concentrations to be 5-10 g/m3, with concentrations ten times larger in the linear features. Through comparison with horizontal thin sections, we could verify that these linear features were brine sheets or layers.

  16. Corrosion product monitoring using an on-line X-ray fluorescence probe

    Energy Technology Data Exchange (ETDEWEB)

    Stauffer, C.C.; Connolly, D.J. [Babcock & Wilcox Research, Alliance, OH (United States); Millett, P. [Electric Power Research Institute, Palo Alto, CA (United States)

    1995-01-01

    The need for monitoring corrosion products is becoming increasingly important as power plants strive to minimize the effects of corrosion products on plant availability. Current methodology for monitoring corrosion products involves collection of samples using membrane filters followed by analysis of the membranes in the laboratory. This technique is labor intensive and provides only average values over lengthy sampling intervals. Recently, a laboratory tool, x-ray fluorescence spectroscopy, has been combined with on-line sampling capability resulting in an on-line instrument capable of measuring iron oxide particulates in a flowing stream at the ppb level and below. After development in the laboratory, the instrument was successfully field tested in a power plant and is currently undergoing a second field test at another plant. This paper will discuss the design and operation of the instrument, and field data obtained from plant service will be presented. Results show that this instrument will provide on-line measurements of iron oxides at the ppb level with minimal operator involvement.

  17. Geochemical analysis of marine sediments using fused glass disc by X-ray fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    XIA Ning; ZHANG Qin; YAO De; LI Guohui

    2008-01-01

    A method was developed for content determination of Na, Mg, Al, Si, P,S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sediment samples using fused glass disc by X-ray Fluorescence spectrometry. Calibration was made using marine sediment certified reference materials and the synthetic standard samples prepared by mixing several marine sediments with stream sediment and carbonate standard samples in different proportions. The matrix effect was corrected using theoretical alpha coefficients, experience coefficients and the scattered radiation as the internal standard (for the trace elements). The accuracy of the method was evaluated by analysis of certified reference materials GBW07314, GBW07334 and GSMS6. The results are in good agreement with the certified values of the standards with RSD less than 2.60%, except for Y, Cr, Ga, Ce, La, Nb, Rb, and V with RSD less than 9.0% (n=12).

  18. Green direct determination of mineral elements in artichokes by infrared spectroscopy and X-ray fluorescence.

    Science.gov (United States)

    Mir-Marqués, Alba; Martínez-García, Maria; Garrigues, Salvador; Cervera, M Luisa; de la Guardia, Miguel

    2016-04-01

    Near infrared (NIR) and X-ray fluorescence (XRF) spectroscopy were investigated to predict the concentration of calcium, potassium, iron, magnesium, manganese and zinc in artichoke samples. Sixty artichokes were purchased from different Spanish areas (Benicarló, Valencia and Murcia). NIR and XRF spectra, combined with partial least squares (PLS) data treatment, were used to develop chemometric models for the prediction of mineral concentration. To obtain reference data, samples were mineralised and analysed by inductively coupled plasma optical emission spectrometry (ICP-OES). Coefficients of determination obtained for the regression between predicted values and reference ones for calcium, potassium, magnesium, iron, manganese and zinc were 0.61, 0.79, 0.53, 0.77, 0.54 and 0.60 for NIR and 0.96, 0.93, 0.80, 0.79, 0.76 and 0.90 for XRF, respectively. Both assayed methodologies, offer green alternatives to classical mineral analysis, but XRF provided the best results in order to be used as a quantitative screening method.

  19. Applications of a glazing incidence X-ray fluorescence analysis to forensic samples

    Energy Technology Data Exchange (ETDEWEB)

    Ninomiya, Toshio [Hyogo Prefecture, Kobe (Japan). Forensic Science Lab.; Nomura, Shigeaki; Taniguchi, Kazuo; Ikeda, Shigero

    1995-06-01

    A glazing incidence X-ray fluorescence analysis (GIXF) has been applied to forensic samples: a counterfeit 100-dollar bill, fragments of polyvinyl tapes, a trace of semen, illegal drugs, fingerprints and fake V.S.O.P brandy. Strontium could not be detected on the magnet-respondent letter of the counterfeit bill and Br was detected on the magnet-nonrespondent part of the counterfeit bill, while such phenomena could not be noticed on a true bill. Fragments of black vinyl tapes related to a sexual assault case could be discriminated from each other. Zinc as a characteristic ingredient could be detected in a trace of semen. Bromine was detected in each of what is called a pure methamphetamine crystal and K, Ca, Fe, Zn etc. were detected in heroin powders. Lead was sharply detected in gunshot residues attached to a finger after gunfiring. Sulfur as a contaminant was abundant in fake V.S.O.P brandy, while no S was detected in genuine V.S.O.P brandy. (author).

  20. Automated nanoliter solution deposition for total reflection X-ray fluorescence analysis of semiconductor samples

    Energy Technology Data Exchange (ETDEWEB)

    Sparks, Chris M. [Process Characterization Laboratory, ATDF, Austin, TX 78741 (United States)]. E-mail: chris.sparks@atdf.com; Gondran, Carolyn H. [Process Characterization Laboratory, ATDF, Austin, TX 78741 (United States); Havrilla, George J. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Hastings, Elizabeth P. [Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2006-11-15

    In this study, a BioDot BioJet dispensing system was investigated as a nanoliter sample deposition method for total reflection X-ray fluorescence (TXRF) analysis. The BioDot system was programmed to dispense arrays of 20 nL droplets of sample solution on Si wafers. Each 20 nL droplet was approximately 100 {mu}m in diameter. A 10 x 10 array (100 droplets) was deposited and dried in less than 2 min at room temperature and pressure, demonstrating the efficiency of the automated deposition method. Solutions of various concentrations of Ni and Ni in different matrices were made from stock trace element standards to investigate of the effect of the matrix on the TXRF signal. The concentrations were such that the levels of TXRF signal saturation could be examined. Arrays were deposited to demonstrate the capability of drying 100 {mu}L of vapor phase decomposition-like residue in the area of a typical TXRF detector.

  1. Hazardous metals in vintage plastic toys measured by a handheld X-ray fluorescence spectrometer.

    Science.gov (United States)

    Miller, Gillian Zaharias; Harris, Zoe E

    2015-01-01

    Over 100 plastic toys from the 1970s and 1980s, both polyvinyl chloride ("vinyl") and nonvinyl, were analyzed in the study described here using a handheld X-ray fluorescence spectrometer to quantify hazardous metal content. A sampling of recent vinyl toys was also tested. The majority of nonvinyl samples were Fisher Price brand toys. The vinyl toys consisted largely of Barbie dolls and other dolls. Overall, lead or cadmium was found in 67% of vintage plastic toys, frequently at concentrations exceeding current U.S. and European limits. Arsenic was detected at levels of concern in 16% of the samples. In the nonvinyl toys, heavy metal content was found to correlate with certain colors of plastic. The likely sources of the detected metals are discussed. None of the contemporary vinyl toys contained detectable cadmium, lead, or arsenic. Given that vintage toys remain in widespread use by children in homes and other locations, the results illuminate a potential source of heavy metal exposure for children.

  2. X-ray Fluorescence Spectroscopy Study of Coating Thickness and Base Metal Composition

    Science.gov (United States)

    Rolin, T. D.; Leszczuk, Y.

    2008-01-01

    For electrical, electronic, and electromechanical (EEE) parts to be approved for space use, they must be able to meet safety standards approved by NASA. A fast, reliable, and precise method is needed to make sure these standards are met. Many EEE parts are coated in gold (Au) and nickel (Ni), and the thickness coating is crucial to a part s performance. A nondestructive method that is efficient in measuring coating thickness is x-ray fluorescence (XRF) spectroscopy. The XRF spectrometer is a machine designed to measure layer thickness and composition of single or multilayered samples. By understanding the limitations in the collection of the data by this method, accurate composition and thickness measurements can be obtained for samples with Au and Ni coatings. To understand the limitations of data found, measurements were taken with the XRF spectrometer and compared to true values of standard reference materials (SRM) that were National Institute of Standards and Technology (NIST) traceable. For every sample, six different parameters were varied to understand measurement error: coating/substrate combination, number of layers, counting interval, collimator size, coating thickness, and test area location. Each measurement was taken in accordance with standards set by the American Society for Testing and Materials (ASTM) International Standard B 568.

  3. X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy analysis of Roman silver denarii

    Energy Technology Data Exchange (ETDEWEB)

    Pardini, L. [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); El Hassan, A. [National Institute for Laser- Enhanced Sciences (NILES), Cairo University Giza (Egypt); Ferretti, M. [Istituto per le Tecnologie Applicate ai Beni Culturali, Area della Ricerca del CNR di Montelibretti Roma (Italy); Foresta, A.; Legnaioli, S.; Lorenzetti, G. [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Nebbia, E. [Universita degli Studi di Torino (Italy); Catalli, F. [Monetiere di Firenze, Museo Archeologico Nazionale Firenze (Italy); Harith, M.A. [National Institute for Laser- Enhanced Sciences (NILES), Cairo University Giza (Egypt); Diaz Pace, D. [Institute of Physics ' Arroyo Seco' , Faculty of Science, Tandil (Argentina); Anabitarte Garcia, F. [Photonics Engineering Group, University of Cantabria, Santander (Spain); Scuotto, M. [Dipartimento di Scienze Archeologiche, Via Galvani 1, 56126 Pisa (Italy); Palleschi, V., E-mail: vincenzo.palleschi@cnr.it [Istituto di Chimica dei Composti Organometallici del CNR, Research Area of Pisa, Via G. Moruzzi 1, 56124 Pisa (Italy); Dipartimento di Scienze Archeologiche, Via Galvani 1, 56126 Pisa (Italy)

    2012-08-15

    In this paper we present the results of a study performed on a large collection of silver Roman republican denarii, encompassing about two centuries of history. The joint use of Laser-Induced Breakdown Spectroscopy (LIBS) and X-Ray Fluorescence (XRF) spectroscopy allowed for an accurate determination of the coins' elemental composition; the measurements, performed mostly in situ at the 'Monetiere' in Florence, revealed a striking connection between the 'quality' of the silver alloy and some crucial contemporary events. This finding was used to classify a group of denarii whose dating was otherwise impossible. The comparison with other contemporary denarii disproves a recent theory on the origin of the so called 'serrated' denarii (denarii showing notched chisel marks on the edge of the coin). - Highlights: Black-Right-Pointing-Pointer We studied a large collection of Roman republican silver denarii. Black-Right-Pointing-Pointer XRF and LIBS allowed to determine the precious metal content of the coins. Black-Right-Pointing-Pointer A correlation of the 'quality' of the alloy with some contemporary events was found. Black-Right-Pointing-Pointer The study allowed to controvert a recent theory on the so called 'serrated' denarii.

  4. Elemental analysis of mining wastes by energy dispersive X-ray fluorescence (EDXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez-Fernandez, O. [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' , CSIC, Sole Sabaris s/n, 08028 Barcelona (Spain)]. E-mail: ogonzalez@ija.csic.es; Queralt, I. [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' , CSIC, Sole Sabaris s/n, 08028 Barcelona (Spain); Carvalho, M.L. [Centro de Fisica Atomica, Universidade de Lisboa, Av. Prof. Gama Pinto, 21649-003 Lisboa (Portugal); Garcia, G. [Area Edafologia y Quimica Agricola, Departmento de Ciencia y Tecnologia Agraria, Universidad Politecnica de Cartagena, Paseo Alfonso XIII 48, 30203 Cartagena (Spain)

    2007-08-15

    An energy dispersive X-ray fluorescence (EDXRF) tri-axial geometry experimental spectrometer has been employed to determine the concentrations of 13 different elements (K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr and Pb) in mine wastes from different depths of two mine tailings from the Cartagena-La Union (Spain) mining district. The elements were determined and quantified using the fundamental parameters method. The concentrations of Cr, Ni, Cu, Zn and Pb were compared to the values from the European and Spanish legislation to evaluate the environmental risk and to classify the wastes as inert wastes or as wastes that have to be control land-filled. The results obtained demonstrate that these wastes can be considered as inert for the considered elements, apart from the concentration levels of Zn and Pb. Whilst Zn slightly overpasses the regulatory levels, Pb mean value exceeds three to six times the value to be considered as Class I potential land-filling material.

  5. The Distribution of Elements in 48 Canine Compact Bone Types Using Handheld X-Ray Fluorescence.

    Science.gov (United States)

    Nganvongpanit, Korakot; Buddhachat, Kittisak; Piboon, Promporn; Klinhom, Sarisa

    2016-11-01

    A major question when we talk about the elements in the bone is whether all bones contain the same elements. To answer this question, this study was designed for determination of the elemental levels in 48 various canine compact bones using handheld X-ray fluorescence technique. From a total of 26 elements that could be detected, only 13 elements were found in all 48 bones. The sternum and os penis were significantly different from the other bones in that they contained the highest number of elements. The ratio of Ca and P was significantly different when comparing certain bones: there was a higher Ca/P ratio in the patella (right), calcaneus (right and left), and sternum compared with a lower ratio in the radius (left), rib (left), phalanx (left forelimb), and carpus (left). These results are the first to demonstrate that different types of bones have different elemental profiles, even for major elements such as Ca and P. Moreover, the Ca/P ratio was also different between bone types. This data is important for the selection of bones appropriate to the element studied. In addition, the results proved that the elements were not equally distributed in every bone in the body.

  6. New applications of the good old wavelength-dispersive X-ray fluorescence

    Indian Academy of Sciences (India)

    Andrzej Kuczumow; Paweł Wolski

    2011-02-01

    Wavelength-dispersive X-ray fluorescence can be characterized by its advantages and drawbacks. Unbeaten spectral resolution in a range below 5 keV, good operational stability, excellent ability of making averaged analysis, and good presentation of peak shape which gives the basis for the chemical speciation are the advantages. Among the drawbacks, the following are important: system with sequential analysis of particular elements, low output of energy supplied to the device, and great cost of instrument which can be amortized only in routine operations. In routine geological and environmental analyses, the WD-XRF performs better than other simpler instrumental or wet techniques. WD-XRF is continuously improved, by applying new multilayer interference mirrors (MIM) for detection and quantification of very light elements. Bad spectral resolution of MIM noted earlier is now improved by tailoring their shape to the shape of gratings. The progress in the long wavelength spectral region joined with efficient and precise wavelength resolution systems enables the application of WD-XRF for speciation analysis. In another effort, XRF spectrometry is treated as a tool for obtaining quantitative basis for the judgement on Linnaean systematic classification of plants and opens the field to a new discipline – quantitative biology.

  7. Evaluation of Field Portable X-Ray Fluorescence Performance for the Analysis of Ni in Soil.

    Science.gov (United States)

    Du, Guo-dong; Lei, Mei; Zhou, Guang-dong; Chen, Tong-bin; Qiu, Rong-liang

    2015-03-01

    As a rapid, in-situ analysis method, Field portable X-ray fluorescence spectrometry (FP-XRF) can be widely applied in soil heavy metals analysis field. Whereas, some factors may affect FP-XRF performance and restrict the application. Studies have proved that FP-XRF has poorer performance when the concentration of target element is low, and soil moisture and particle size will affect FP-XRF performance. But few studies have been conducted in depth. This study took an example of Ni, demonstrated the relationship between Ni concentration and FP-XRF performance on accuracy and precision, and gave a critical value. Effects of soil moisture and particle size on accuracy and precision also had been compared. Results show that, FP-XRF performance is related to Ni concentration and the critical value is 400 mg x kg(-1). Relative standard deviation (RSD) and relative uncertainty decrease while the Ni concentration is below 400 mg x kg(-1), hence FP-XRF performance improves with increasing Ni concentration in this range; RSD and relative uncertainty change little while the Ni concentration is above 400 mg x kg(-1), hence FP-XRF performance does not have correlation with Ni concentration any more. For in-situ analysis, the relative uncertainty contributed by soil moisture is 3.77%, and the relative certainty contributed by particle size is 0.56%. Effect of soil moisture is evidently more serious than particle size both on accuracy and precision.

  8. Total reflection X-ray fluorescence analysis of pollen as an indicator for atmospheric pollution*1

    Science.gov (United States)

    Pepponi, G.; Lazzeri, P.; Coghe, N.; Bersani, M.; Gottardini, E.; Cristofolini, F.; Clauser, G.; Torboli, A.

    2004-08-01

    The viability of pollen is affected by environmental pollution and its use as a bio-indicator is proposed. Such effects can be observed and quantified by biological tests. However, a more accurate identification of the agents affecting the viability is required in order to validate the biological assay for environmental monitoring. The chemical analysis of pollen is meant to ascertain the existence of a correlation between its reduced biological functions and the presence of pollutants. Moreover, such biological systems act as accumulators and allow the detection and quantification of species present in the environment at low concentrations. Total reflection X-ray fluorescence analysis (TXRF) has been chosen for the investigation due to its high sensitivity, multielement capability and wide dynamic range. Corylus avellana L. (hazel) pollen has been collected in areas with different anthropic impact in the province of Trento, Italy. For the TXRF measurements, a liquid sample is needed, especially if a quantitative analysis is required. In the present work, the analysis after a microwave digestion has been compared with the analysis of a suspension of the pollen samples. In both cases, an internal standard has been used for the quantification. The concentrations of 17 elements ranging from Al to Pb have been determined in 13 samples. Analysis of the suspensions showed to be comparable to that of digested samples in terms of spectral quality, but the latter preparation method gave better reproducibility. Sub-ppm lowest limits of detection were obtained for iron and heavier elements detected.

  9. Determination of metals in air samples using X-Ray fluorescence associated the APDC preconcentration technique

    Energy Technology Data Exchange (ETDEWEB)

    Nardes, Raysa C.; Santos, Ramon S.; Sanches, Francis A.C.R.A.; Gama Filho, Hamilton S.; Oliveira, Davi F.; Anjos, Marcelino J., E-mail: rc.nardes@gmail.com, E-mail: ramonziosp@yahoo.com.br, E-mail: francissanches@gmail.com, E-mail: hamiltongamafilho@hotmail.com, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Fisica. Departamento de Fisica Aplicada e Termodinamica

    2015-07-01

    Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public / cultural patrimonies. The inhalable particulate materials can cause the emergence and / or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus, preconcentration with APDC and Total Reflection X-ray Fluorescence technique (TXRF) to analyze the heavy metals present in the air. The samples were collected from five random points in the city of Rio de Janeiro/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic. (author)

  10. Quantitative comparison of preparation methodologies for X-ray fluorescence microscopy of brain tissue

    Energy Technology Data Exchange (ETDEWEB)

    James, Simon A.; Sexton, Brett A.; Hoobin, Pamela; Mayo, Sheridan C. [CSIRO, Materials Science and Engineering and the Preventative Health Flagship, Clayton, VIC (Australia); Myers, Damian E. [St. Vincent s Hospital, Department of Surgery/Orthopaedics, Fitzroy, VIC (Australia); University of Melbourne, Department of Surgery, Parkville, VIC (Australia); Jonge, Martin D. de; Paterson, David; Howard, Daryl L. [Australian Synchrotron, Clayton, VIC (Australia); Vogt, Stefan [Argonne National Laboratory, X-ray Science Division, Argonne, IL (United States); Ryan, Chris G. [CSIRO, Earth Science and Resources Engineering, Clayton, VIC (Australia); University of Melbourne, School of Physics, Parkville, VIC (Australia); University of Tasmania, CODES Centre of Excellence, Hobart, TAS (Australia); Altissimo, Matteo [Melbourne Centre for Nanofabrication, Clayton, VIC (Australia); Moorhead, Gareth F. [CSIRO, Materials Science and Engineering and the Preventative Health Flagship, Clayton, VIC (Australia); University of Melbourne, School of Physics, Parkville, VIC (Australia); Wilkins, Stephen W. [CSIRO, Materials Science and Engineering and the Preventative Health Flagship, Clayton, VIC (Australia); Monash University, School of Physics, Clayton, VIC (Australia)

    2011-08-15

    X-ray fluorescence microscopy (XFM) facilitates high-sensitivity quantitative imaging of trace metals at high spatial resolution over large sample areas and can be applied to a diverse range of biological samples. Accurate determination of elemental content from recorded spectra requires proper calibration of the XFM instrument under the relevant operating conditions. Here, we describe the manufacture, characterization, and utilization of multi-element thin-film reference foils for use in calibration of XFM measurements of biological and other specimens. We have used these internal standards to assess the two-dimensional distribution of trace metals in a thin tissue section of a rat hippocampus. The data used in this study was acquired at the XFM beamline of the Australian Synchrotron using a new 384-element array detector (Maia) and at beamline 2-ID-E at the Advanced Photon Source. Post-processing of samples by different fixation techniques was investigated, with the conclusion that differences in solvent type and sample handling can significantly alter elemental content. The present study highlights the quantitative capability, high statistical power, and versatility of the XFM technique for mapping trace metals in biological samples, e.g., brain tissue samples in order to help understand neurological processes, especially when implemented in conjunction with a high-performance detector such as Maia. (orig.)

  11. Preparation of specimens for analysis by: X-ray diffraction and X-ray fluorescence analysis; Preparacion de especimenes para analisis por: Difraccion de rayos X y Fluorescencia de rayos X

    Energy Technology Data Exchange (ETDEWEB)

    Banos L, L. [IIM, UNAM, A.P. 70-360, 04510 Mexico D.F. (Mexico)

    2004-07-01

    Specimen preparation is one of the most important requirements in the analysis of samples by X-ray Diffraction and X-ray Fluorescence. This statement is especially true for samples containing different types of materials. There are many forms of specimen suitable for X-ray analysis and the type of the sample as received will generally determine the method of pretreatment. It is convenient to refer to the material received for analysis as the sample, and that, which is actually analyzed as the specimen. The powder Diffraction method assumes that the particles in the specimen are ideally random orientation and that there are enough crystallites in the specimen to achieve a representative intensity distribution for these crystallites. X ray Fluorescence is essentially a comparative method of analysis, it is vital that all standards and unknowns be presented to the spectrometer in a reproducible and identical manner. (Author) 3 refs., 6 figs.

  12. Element distribution in the brain sections of rats measured by synchrotron radiation X-ray fluorescence

    Science.gov (United States)

    Liu, N. Q.; Zhang, F.; Wang, X. F.; Zhang, Z. Y.; Chai, Z. F.; Huang, Y. Y.; He, W.; Zhao, X. Q.; Zuo, A. J.; Yang, R.

    2004-02-01

    The concentration of trace elements in brain sections was measured by synchrotron radiation X-ray fluorescence. The relative concentration was calculated by means of the normalization of Compton scattering intensity approximately 22 keV, after the normalization for collecting time of X-ray spectrum and the counting of the ion chamber, and subtracting the contribution of the polycarbonate film for supporting sample. Furthermore, the statistical evaluation of the element distribution in various regions of the brain sections of the 20-day-old rats was tested. For investigating the distribution of elements in the brain of iodine deficient rats, Wistar rats were fed with iodine deficient diet and deionized water (ID group). The rats were fed the same iodine deficient diet, but drank KIO 3 solution as control (CT group). The results showed that the contents of calcium (Ca) in thalamus (TH) and copper (Cu) and iron (Fe) in cerebral cortex (CX) of ID rats were significantly lower than that of control rats, while the contents of phosphor (P), sulfur (S), potassium (K), rubidium (Rb), bromine (Br), chlorine (Cl), zinc (Zn), Ca and Cu of ID in hippocampus (H) and the contents of Br, Cl, Zn and Ca in cerebral cortex of ID rats were significantly higher. Especially, the difference of Br, Cl, Zn and Ca in H between ID and CT was more significant. The contents of all elements measured in H were higher than (or equal to) CX and/or TH for both groups, except low Cl of the control rats. Furthermore Zn and Cu contents along the hippocampal fissure in both groups were 1.5 ( Ptimes higher than in hippocampus, respectively. Considering the results of cluster analysis our study shows that the marked alterations in the spatial distribution of Zn and Ca of ID rats brain during brain development stages. In addition, the effect of the perfusion with 0.9% NaCl solution before taking brain on the distribution of elements in the brain sections was observed and discussed.

  13. Iodinated silica/porphyrin hybrid nanoparticles for X-ray computed tomography/fluorescence dual-modal imaging of tumors

    Directory of Open Access Journals (Sweden)

    Koichiro Hayashi

    2014-12-01

    Full Text Available Silica nanoparticles containing covalently linked iodine and a near-infrared (NIR fluorescence dye, namely porphyrin, have been synthesized through a one-pot sol–gel reaction. These particles are called iodinated silica/porphyrin hybrid nanoparticles (ISP HNPs. The ISP HNPs have both high X-ray absorption coefficient and NIR fluorescence. The ISP HNPs modified with folic acid (FA and polyethylene glycol (PEG, denoted as FA-PEG-ISP HNPs, enabled the successful visualization of tumors in mice by both X-ray computed tomography (CT and fluorescence imaging (FI. Thus, the FA-PEG-ISP HNPs are useful as contrast agents or probes for CT/FI dual-modal imaging.

  14. Structural Basis of X-ray-Induced Transient Photo-bleaching in a Photoactivatable Green Fluorescent Protein

    Energy Technology Data Exchange (ETDEWEB)

    Adam, V. [European Synchrotron Radiation Facility, 6 rue Jules Horowitz, BP 220, 38043 Grenoble Cedex (France); Carpentier, Ph.; Lelimousin, M.; Darnault, C.; Bourgeois, D. [IBS, Institut de Biologie Structurale Jean-Pierre Ebel, CEA, CNRS, UniVersite Joseph Fourier, 41 rue Jules Horowitz, 38027 Grenoble (France); Violot, S. [Laboratoire de Physiologie Cellulaire Vegetale, Institut de Recherches en Technologie et Sciences pour le ViVant, CEA, CNRS, INRA, UniVersite Joseph Fourier, 17 rue des Martyrs, F-38054 Grenoble (France); Nienhaus, U. [Institute of Applied Physics and Center for Functional nano-structures (CFN), Karlsruhe Institute of Technology, 76128 Karlsruhe (Germany); Nienhaus, U. [Department of Physics, UniVersity of Illinois at Urbana-Champaign, Urbana, Illinois 61801 (US)

    2009-07-01

    We have observed the photoactivatable fluorescent protein IrisFP in a transient dark state with near-atomic resolution. This dark state is assigned to a radical species that either relaxes to the ground state or evolves into a permanently bleached chromophore. We took advantage of X-rays to populate the radical, which presumably forms under illumination with visible light by an electron-transfer reaction in the triplet state. The combined X-ray diffraction and in crystallo UV-vis absorption, fluorescence, and Raman data reveal that radical formation in IrisFP involves pronounced but reversible distortion of the chromophore, suggesting a transient loss of {pi} conjugation. These results reveal that the methylene bridge of the chromophore is the Achilles' heel of fluorescent proteins and help unravel the mechanisms of blinking and photo-bleaching in FPs, which are of importance in the rational design of photo-stable variants. and is also partly reversible. (authors)

  15. X-ray fluorescence imaging: a new tool for studying manganese neurotoxicity.

    Directory of Open Access Journals (Sweden)

    Gregory Robison

    Full Text Available The neurotoxic effect of manganese (Mn establishes itself in a condition known as manganism or Mn induced parkinsonism. While this condition was first diagnosed about 170 years ago, the mechanism of the neurotoxic action of Mn remains unknown. Moreover, the possibility that Mn exposure combined with other genetic and environmental factors can contribute to the development of Parkinson's disease has been discussed in the literature and several epidemiological studies have demonstrated a correlation between Mn exposure and an elevated risk of Parkinson's disease. Here, we introduce X-ray fluorescence imaging as a new quantitative tool for analysis of the Mn distribution in the brain with high spatial resolution. The animal model employed mimics deficits observed in affected human subjects. The obtained maps of Mn distribution in the brain demonstrate the highest Mn content in the globus pallidus, the thalamus, and the substantia nigra pars compacta. To test the hypothesis that Mn transport into/distribution within brain cells mimics that of other biologically relevant metal ions, such as iron, copper, or zinc, their distributions were compared. It was demonstrated that the Mn distribution does not follow the distributions of any of these metals in the brain. The majority of Mn in the brain was shown to occur in the mobile state, confirming the relevance of the chelation therapy currently used to treat Mn intoxication. In cells with accumulated Mn, it can cause neurotoxic action by affecting the mitochondrial respiratory chain. This can result in increased susceptibility of the neurons of the globus pallidus, thalamus, and substantia nigra pars compacta to various environmental or genetic insults. The obtained data is the first demonstration of Mn accumulation in the substantia nigra pars compacta, and thus, can represent a link between Mn exposure and its potential effects for development of Parkinson's disease.

  16. X-Ray Fluorescence Analysis of XII–XIV Century Italian Gold Coins

    Directory of Open Access Journals (Sweden)

    Monica Baldassarri

    2014-01-01

    Full Text Available An extensive analytical study has been performed on a large number of gold coins (Norman-Swabian Augustale and Tarì, Grosso of Lucca, Florin of Florence minted in Italy from the end of XII century to XIV century. The X-ray fluorescence (XRF technique was used for verifying the composition of the coins. XRF is a nondestructive technique particularly suited for in situ quantitative analysis of gold and minor elements in the precious alloy. The Florins turned out to have a gold content very close to 24 carats (pure gold although in a couple of cases we observed relatively high concentrations of iron (around 2% or lead (around 1%. The Grosso of Lucca has a similar composition, with a measured gold content around 97% due to a higher silver percentage (about 2%, with respect to the average Florin. The Augustali analyzed showed, on average, a gold content around 89%. The average gold content of the Tarì analysed is around 72%, with a relatively large variability. The analysis revealed the use of native gold for the coinage of the Florins, excluding the possibility of recycling gold coming from other sources. On the other hand, the variability observed in the compositions of the Tarì and Augustali could suggest the reuse of Islamic and North African gold. The study could shed some light on the sudden diffusion of gold coins in Italy around the first half of XIII century, allowing hypotheses on the provenience of the gold used for a coinage that dominated the economic trades from then on.

  17. Perspectives on heterococcolith geochemical proxies based on high-resolution X-ray fluorescence mapping.

    Science.gov (United States)

    Suchéras-Marx, B; Giraud, F; Simionovici, A; Daniel, I; Tucoulou, R

    2016-07-01

    Heterococcoliths are micron-scale calcite platelets produced by coccolithophores. They have been the most abundant and continuous fossil record over the last 215 million years (Myr), offering great potential for geochemical studies, although the heterococcolith fossil record remains underutilised in this domain. We have mapped heterococcoliths' composition using X-ray fluorescence (XRF) with a 100-nm resolution beam to decipher element distributions in heterococcoliths and to investigate the potential development of geochemical proxies for palaeoceanography. The study presents two Middle Jurassic Watznaueria britannica heterococcoliths from Cabo Mondego, Portugal. XRF analysis was performed with a 17 keV incident energy beam at the European Synchrotron Radiation Facility ID22NI beamline to study elements from Sr down to S. Ca, Sr and Mn are distributed following the heterococcolith crystalline arrangement. Cl, Br and S display an homogeneous distribution, whereas K, Fe, Cu, Zn and Rb are concentrated at the edges and in the central area of the heterococcoliths. Distributions of K, Fe, Ti, Fe, Cu, Zn, Rb and to a lesser extent V and Cr are highly influenced by clay contamination and peripheral diagenetic overgrowth. Mn is related to diagenetic Mn-rich CaCO3 overgrowth on top of or between heterococcoliths shields. Cl and Br are likely to be present in heterococcoliths inside interstitial nano-domains. We assume that the cytoplasm [Cl(-) ] and [Br(-) ] are mediated and constant during heterococcolithogenesis. Assuming a linear correlation between cytoplasm [Cl(-) ] and sea water [Cl(-) ], heterococcolith Cl may have potential as a salinity proxy. As S is incorporated into heterococcoliths by sulphated polysaccharides, our study suggests a role for such polysaccharides in heterococcolithogenesis for at least 170 Myr. The low Sr/Ca in the W. britannica specimens studied here may either highlight an unusual cellular physiology of Mesozoic coccolithophores or result

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-06-15

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

  19. Study of decorated archeological ceramics by micro X-ray fluorescence spectroscopy

    Science.gov (United States)

    Papadopoulou, D.; Sakalis, A.; Merousis, N.; Tsirliganis, N. C.

    2007-09-01

    Micro-X-ray fluorescence (μ-XRF) spectrometry is an analytical technique that is especially suitable for the study of archeological findings since it is non-destructive, rapid, universal, versatile and multi-elemental. In the present work a compact portable μ-XRF spectrometer was used to characterize decorated sherds of Neolithic pottery from Polyplatanos, North Greece. The sherds were divided into four decorative groups (crusted, classic Dimini, cream on red, and black on red) and the characterization was focused on the determination of certain major, minor and trace elements (Si, K, Ca, Ti, Cr, Mn, Fe, Ni) on the decorated surface and in the clay body. The aim of this characterization was to supplement and confirm archeological information regarding the origin of the artifacts and the manufacturing techniques used for their production. The most predominant chemical elements were determined, and representative ratios (Ca/K, Fe/Mn) were calculated and compared for each individual sample group. The crusted samples and the cream on red samples showed higher concentrations of Ca in the white-crusted surface in comparison with the clay body while Fe was the predominant element in the red decorated surface. The analysis of the samples of classic Dimini, revealed higher concentrations of Mn in the black painted surfaces and higher Ca content in the light-coloured clay bodies. Finally, most samples of the black on red group present high concentrations of Mn in their decoration surface. Zn and Ni were also detected in this group in contrast with the remaining groups.

  20. Visualizing Metal Content and Intracellular Distribution in Primary Hippocampal Neurons with Synchrotron X-Ray Fluorescence

    Science.gov (United States)

    2016-01-01

    Increasing evidence suggests that metal dyshomeostasis plays an important role in human neurodegenerative diseases. Although distinctive metal distributions are described for mature hippocampus and cortex, much less is known about metal levels and intracellular distribution in individual hippocampal neuronal somata. To solve this problem, we conducted quantitative metal analyses utilizing synchrotron radiation X-Ray fluorescence on frozen hydrated primary cultured neurons derived from rat embryonic cortex (CTX) and two regions of the hippocampus: dentate gyrus (DG) and CA1. Comparing average metal contents showed that the most abundant metals were calcium, iron, and zinc, whereas metals such as copper and manganese were less than 10% of zinc. Average metal contents were generally similar when compared across neurons cultured from CTX, DG, and CA1, except for manganese that was larger in CA1. However, each metal showed a characteristic spatial distribution in individual neuronal somata. Zinc was uniformly distributed throughout the cytosol, with no evidence for the existence of previously identified zinc-enriched organelles, zincosomes. Calcium showed a peri-nuclear distribution consistent with accumulation in endoplasmic reticulum and/or mitochondria. Iron showed 2–3 distinct highly concentrated puncta only in peri-nuclear locations. Notwithstanding the small sample size, these analyses demonstrate that primary cultured neurons show characteristic metal signatures. The iron puncta probably represent iron-accumulating organelles, siderosomes. Thus, the metal distributions observed in mature brain structures are likely the result of both intrinsic neuronal factors that control cellular metal content and extrinsic factors related to the synaptic organization, function, and contacts formed and maintained in each region. PMID:27434052

  1. Effects of amiodarone therapy on thyroid iodine content as measured by x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Fragu, P.; Schlumberger, M.; Davy, J.M.; Slama, M.; Berdeaux, A.

    1988-04-01

    Thyroid iodine content (TIC) was measured by x-ray fluorescence in 68 patients who had received amiodarone treatment for varying intervals (1 g/week for 1-120 months). Thirty-six patients were euthyroid; the mean TIC of the patients (n = 15), who had been treated for less than 12 months was 30 +/- 19 (+/- SD) mg, twice the normal mean value (14.6 +/- 5.0 mg), and it was 39 +/- 17 mg in those (n = 16) who had been treated for 12-60 months and 29 +/- 6 mg in those (n = 5) who had been treated longer (greater than 60 months). Nineteen patients were hyperthyroid and had elevated TIC values. Of them, 6 patients had a goiter; their TIC (50 +/- 19 mg) was not significantly different from that of the hyperthyroid patients with no goiter (55 +/- 29 mg), but they became hyperthyroid more rapidly. Thirteen patients were hypothyroid; none had TIC values above the normal range, and it was below 2.5 mg in 5 patients. A sequential study was undertaken in 11 euthyroid patients who had no detectable antithyroid antibodies. TIC did not increase during treatment in 2 patients; both developed hypothyroidism, which was transient in 1 despite continuation of amiodarone treatment. The TIC initially increased during amiodarone treatment in the other 9 patients, leveling off at the end of the first year. The TIC rose well above the upper limit of the normal range in 4 patients, of whom 2 became hyperthyroid during the second year of treatment. TIC remained within the normal range in the other 5 patients, of whom 3 became hypothyroid after 12-24 months of treatment (1 subclinical, 2 overt). Although the TIC was significantly higher in the patients with hyperthyroidism than in the patients who remained euthyroid, the TIC test cannot be used to predict the occurrence of hyperthyroidism.

  2. Study of decorated archeological ceramics by micro X-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Papadopoulou, D. [Archaeometry Laboratory, Cultural and Educational Technology Institute/R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece); Technological Educational Institute of Kavala, Department of Science, Agios Loukas, 654 04 Kavala (Greece); Sakalis, A. [Archaeometry Laboratory, Cultural and Educational Technology Institute/R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece)], E-mail: asakalis@ceti.gr; Merousis, N. [Hellenic Open University, Kyzikou 25-27, 55133 Kalamaria, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute/R.C. ' Athena' , Tsimiski 58, 67100 Xanthi (Greece)

    2007-09-21

    Micro-X-ray fluorescence ({mu}-XRF) spectrometry is an analytical technique that is especially suitable for the study of archeological findings since it is non-destructive, rapid, universal, versatile and multi-elemental. In the present work a compact portable {mu}-XRF spectrometer was used to characterize decorated sherds of Neolithic pottery from Polyplatanos, North Greece. The sherds were divided into four decorative groups (crusted, classic Dimini, cream on red, and black on red) and the characterization was focused on the determination of certain major, minor and trace elements (Si, K, Ca, Ti, Cr, Mn, Fe, Ni) on the decorated surface and in the clay body. The aim of this characterization was to supplement and confirm archeological information regarding the origin of the artifacts and the manufacturing techniques used for their production. The most predominant chemical elements were determined, and representative ratios (Ca/K, Fe/Mn) were calculated and compared for each individual sample group. The crusted samples and the cream on red samples showed higher concentrations of Ca in the white-crusted surface in comparison with the clay body while Fe was the predominant element in the red decorated surface. The analysis of the samples of classic Dimini, revealed higher concentrations of Mn in the black painted surfaces and higher Ca content in the light-coloured clay bodies. Finally, most samples of the black on red group present high concentrations of Mn in their decoration surface. Zn and Ni were also detected in this group in contrast with the remaining groups.

  3. Visualizing Metal Content and Intracellular Distribution in Primary Hippocampal Neurons with Synchrotron X-Ray Fluorescence.

    Directory of Open Access Journals (Sweden)

    Robert A Colvin

    Full Text Available Increasing evidence suggests that metal dyshomeostasis plays an important role in human neurodegenerative diseases. Although distinctive metal distributions are described for mature hippocampus and cortex, much less is known about metal levels and intracellular distribution in individual hippocampal neuronal somata. To solve this problem, we conducted quantitative metal analyses utilizing synchrotron radiation X-Ray fluorescence on frozen hydrated primary cultured neurons derived from rat embryonic cortex (CTX and two regions of the hippocampus: dentate gyrus (DG and CA1. Comparing average metal contents showed that the most abundant metals were calcium, iron, and zinc, whereas metals such as copper and manganese were less than 10% of zinc. Average metal contents were generally similar when compared across neurons cultured from CTX, DG, and CA1, except for manganese that was larger in CA1. However, each metal showed a characteristic spatial distribution in individual neuronal somata. Zinc was uniformly distributed throughout the cytosol, with no evidence for the existence of previously identified zinc-enriched organelles, zincosomes. Calcium showed a peri-nuclear distribution consistent with accumulation in endoplasmic reticulum and/or mitochondria. Iron showed 2-3 distinct highly concentrated puncta only in peri-nuclear locations. Notwithstanding the small sample size, these analyses demonstrate that primary cultured neurons show characteristic metal signatures. The iron puncta probably represent iron-accumulating organelles, siderosomes. Thus, the metal distributions observed in mature brain structures are likely the result of both intrinsic neuronal factors that control cellular metal content and extrinsic factors related to the synaptic organization, function, and contacts formed and maintained in each region.

  4. Evaluation of a novel portable x-ray fluorescence screening tool for detection of arsenic exposure.

    Science.gov (United States)

    McIver, David J; VanLeeuwen, John A; Knafla, Anthony L; Campbell, Jillian A; Alexander, Kevin M; Gherase, Mihai R; Guernsey, Judith R; Fleming, David E B

    2015-12-01

    A new portable x-ray fluorescence (XRF) screening tool was evaluated for its effectiveness in arsenic (As) quantification in human finger and toe nails ([Formula: see text]). Nail samples were measured for total As concentration by XRF and inductively coupled plasma-mass spectrometry (ICP-MS). Using concordance correlation coefficient (CCC), kappa, diagnostic sensitivity (Sn) and specificity (Sp), and linear regression analyses, the concentration of As measured by XRF was compared to ICP-MS. The CCC peaked for scaled values of fingernail samples, at 0.424 (95% CI: 0.065-0.784). The largest kappa value, 0.400 (95% CI:  -0.282-1.000), was found at a 1.3 μg g(-1) cut-off concentration, for fingernails only, and the largest kappa at a clinically relevant cut-off concentration of 1.0 μg g(-1) was 0.237 (95% CI:  -0.068-0.543), again in fingernails. Analyses generally showed excellent XRF Sn (up to 100%, 95% CI: 48-100%), but low Sp (up to 30% for the same analysis, 95% CI: 14-50%). Portable XRF shows some potential for use as a screening tool with fingernail samples. The difference between XRF and ICP-MS measurements decreased as sample mass increased to 30 mg. While this novel method of As detection in nails has shown relatively high agreement in some scenarios, this portable XRF is not currently considered suitable as a substitute for ICP-MS.

  5. Analysis of limestones and dolomites by x-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Wheeler, B.D.

    1999-07-01

    Sources of calcium are generally widespread and quite extensive. These sources are limestone, dolomite, marl, chalk, and oyster shell. Cement plants account for nearly half of the demand, while two hundred lime plants in the US and Puerto Rico consume about twenty five percent. Since the chemical composition of the limestone and other sources of calcium is critical in the cement and lime industry, particularly for the deleterious compounds such as sodium oxide, Na{sub 2}O, magnesium oxide, MgO, phosphorus pentoxide, P{sub 2}O{sub 5}, and potassium oxide, K{sub 2}O, accurate determinations are critical. Due to the tonnage per hour, these determinations must be made rapidly and accurately. X-ray fluorescence can thereby satisfy this need for accuracy and also precision. Production of lime is performed by calcining limestone or dolomite in which the industry is generally located and concentrated in the States of Michigan and Pennsylvania. The resulting product is quicklime, CaO, and hydrated lime, Ca(OH){sub 2}. Substantial amounts of quicklime is further processed into calcium carbide in order to produce acetylene gas. In this case, the determination of P{sub 2}O{sub 5} is critical since minor quantities of phosphorus in acetylene gas can cause premature explosions. Other uses for lime are well known in the treatment of water, the paper and pulp industry, and in the steel industry for the production of slag to remove impurities. Dolomitic lime is heavily utilized in the manufacture of magnesite refractories by reacting dolomitic lime with brines from the Michigan Basin to produce magnesium oxide, MgO, and calcium chloride, CaCl{sub 2}. Sample preparation for these materials usually is performed by grinding and pelletizing or fusion with lithium-tetra-borate, Li{sub 2}B{sub 4}O{sub 7}.

  6. Pb distribution in bones from the Franklin expedition: synchrotron X-ray fluorescence and laser ablation/mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Ronald Richard; Naftel, Steven; Macfie, Sheila; Jones, Keith; Nelson, Andrew [The University of Western Ontario, London, ON (Canada)

    2013-04-15

    Synchrotron micro-X-ray Fluorescence has been used to map the metal distribution in selected bone fragments representative of remains associated with the Franklin expedition. In addition, laser ablation mass spectroscopy using a 25 {mu}m diameter circular spot was employed to compare the Pb isotope distributions in small regions within the bone fragments. The X-ray Fluorescence mapping shows Pb to be widely distributed in the bone while the Pb isotope ratios obtained by laser ablation within small areas representative of bone with different Pb exchange rates do not show statistically significant differences. These results are inconsistent with the hypothesis that faulty solder seals in tinned meat were the principle source of Pb in the remains of the expedition personnel. (orig.)

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

    Science.gov (United States)

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

    2011-01-01

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

  8. Fluorescence imaging of reactive oxygen species by confocal laser scanning microscopy for track analysis of synchrotron X-ray photoelectric nanoradiator dose: X-ray pump-optical probe.

    Science.gov (United States)

    Jeon, Jae Kun; Han, Sung Mi; Kim, Jong Ki

    2016-09-01

    Bursts of emissions of low-energy electrons, including interatomic Coulomb decay electrons and Auger electrons (0-1000 eV), as well as X-ray fluorescence produced by irradiation of large-Z element nanoparticles by either X-ray photons or high-energy ion beams, is referred to as the nanoradiator effect. In therapeutic applications, this effect can damage pathological tissues that selectively take up the nanoparticles. Herein, a new nanoradiator dosimetry method is presented that uses probes for reactive oxygen species (ROS) incorporated into three-dimensional gels, on which macrophages containing iron oxide nanoparticles (IONs) are attached. This method, together with site-specific irradiation of the intracellular nanoparticles from a microbeam of polychromatic synchrotron X-rays (5-14 keV), measures the range and distribution of OH radicals produced by X-ray emission or superoxide anions ({\\rm{O}}_2^-) produced by low-energy electrons. The measurements are based on confocal laser scanning of the fluorescence of the hydroxyl radical probe 2-[6-(4'-amino)phenoxy-3H-xanthen-3-on-9-yl] benzoic acid (APF) or the superoxide probe hydroethidine-dihydroethidium (DHE) that was oxidized by each ROS, enabling tracking of the radiation dose emitted by the nanoradiator. In the range 70 µm below the irradiated cell, ^\\bullet{\\rm{OH}} radicals derived mostly from either incident X-ray or X-ray fluorescence of ION nanoradiators are distributed along the line of depth direction in ROS gel. In contrast, {\\rm{O}}_2^- derived from secondary electron or low-energy electron emission by ION nanoradiators are scattered over the ROS gel. ROS fluorescence due to the ION nanoradiators was observed continuously to a depth of 1.5 mm for both oxidized APF and oxidized DHE with relatively large intensity compared with the fluorescence caused by the ROS produced solely by incident primary X-rays, which was limited to a depth of 600 µm, suggesting dose enhancement as well as more

  9. Evaluation on the stability of Hg in ABS disk CRM during measurements by wavelength dispersive X-ray fluorescence spectrometry.

    Science.gov (United States)

    Ohata, Masaki; Kidokoro, Toshihiro; Hioki, Akiharu

    2012-01-01

    The stability of Hg in an acrylonitrile-butadiene-styrene disk certified reference material (ABS disk CRM, NMIJ CRM 8116-a) during measurements by wavelength dispersion X-ray fluorescence (WD-XRF) analysis was evaluated in this study. The XRF intensities of Hg (L(α)) and Pb (L(α)) as well as the XRF intensity ratios of Hg (L(α))/Pb (L(α)) observed under different X-ray tube current conditions as well as their irradiation time were examined to evaluate the stability of Hg in the ABS disk CRM. The observed XRF intensities and the XRF intensity ratios for up to 32 h of measurements under 80 mA of X-ray tube current condition were constant, even though the surface of the ABS disk CRM was charred by the X-ray irradiation with high current for a long time. Moreover, the measurements on Hg and Pb in the charred disks by an energy dispersive XRF (ED-XRF) spectrometer showed constant XRF intensity ratios of Hg (L(α))/Pb (L(α)). From these results, Hg in the ABS disk CRM was evaluated to be sufficiently stable for XRF analysis.

  10. X-RAY FLUORESCENCE ANALYSIS OF HANFORD LOW ACTIVITY WASTE SIMULANTS

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-05-08

    Savannah River National Laboratory (SRNL) was requested to develop an x-ray fluorescence (XRF) spectrometry method for elemental characterization of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) pretreated low activity waste (LAW) stream to the LAW Vitrification Plant. The WTP is evaluating the potential for using XRF as a rapid turnaround technique to support LAW product compliance and glass former batching. The overall objective of this task was to develop XRF analytical methods that provide the rapid turnaround time (<8 hours) requested by the WTP, while providing sufficient accuracy and precision to determine waste composition variations. For Phase 1a, SRNL (1) evaluated, selected, and procured an XRF instrument for WTP installation, (2) investigated three XRF sample methods for preparing the LAW sub-sample for XRF analysis, and (3) initiated scoping studies on AN-105 (Envelope A) simulant to determine the instrument's capability, limitations, and optimum operating parameters. After preliminary method development on simulants and the completion of Phase 1a activities, SRNL received approval from WTP to begin Phase 1b activities with the objective of optimizing the XRF methodology. Three XRF sample methods used for preparing the LAW sub-sample for XRF analysis were studied: direct liquid analysis, dried spot, and fused glass. The direct liquid method was selected because its major advantage is that the LAW can be analyzed directly without any sample alteration that could bias the method accuracy. It also is the fastest preparation technique--a typical XRF measurement could be completed in < 1hr after sample delivery. Except for sodium, the method detection limits (MDLs) for the most important analytes in solution, the hold point elements, were achieved by this method. The XRF detection limits are generally adequate for glass former batching and product composition reporting, but may be inadequate for some species (Hg, Cd, and Ba) important

  11. Characterization of urban air pollution by total reflection X-ray fluorescence*1

    Science.gov (United States)

    Schmeling, Martina

    2004-08-01

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

  12. Quantitative Chemical Analysis of Archaeological Slag Material Using Handheld X-ray Fluorescence Spectrometry.

    Science.gov (United States)

    Scott, Rebecca B; Eekelers, Kim; Degryse, Patrick

    2016-01-01

    Handheld X-ray fluorescence spectrometry (XRF) has seen a dramatic increase in use for archaeological projects. The attraction of the technique is its portable and nondestructive nature. In many cases, the archaeological artefacts in question cannot be destructively sampled, or the piece itself cannot be sent to an analytical laboratory. One of the current research interests associated with the Sagalassos project is the study of the Roman iron industry. Previously exported iron slag and ore from the site and the surrounding area was subjected to laboratory chemical analyses. These indicated that different ores were being utilized in the production of iron in different periods. In order to further the project the slag material still in the site depot needed to be analyzed. However, recent legislative changes mean that materials can only be analyzed on-site. Since samples could not be taken and destructive chemical analysis was no longer feasible, a portable, nondestructive technique was required. Handheld XRF can easily provide qualitative data, but these data are only comparable to other handheld XRF qualitative data, from the same device. Quantitative data gathering is possible, but can be more problematic, particularly when the material in question is heterogeneous in nature. A calibration file was created using the manufacturer's software and "in-house" standards made from the pre-quantified samples of iron slag available in the laboratory. In order to make the calibration as robust as possible, the composition of the standards was analyzed statistically to determine which of these created bias and leverage for specific elements. These standards were then omitted from the calibration for that element. The calibration was tested in the laboratory using samples of iron slag previously analyzed with wet chemistry, and the results indicated that most sample analyses showed 30% error were found in samples which contained very low or very high quantities of the

  13. Selenium Preferentially Accumulates in the Eye Lens Following Embryonic Exposure: A Confocal X-ray Fluorescence Imaging Study

    Energy Technology Data Exchange (ETDEWEB)

    Choudhury, Sanjukta; Thomas, Jith; Sylvain, Nicole J.; Ponomarenko, Olena; Gordon, Robert A.; Heald, Steve M.; Janz, David M.; Krone, Patrick H.; Coulthard, Ian; George, Graham N.; Pickering, Ingrid J.

    2015-02-17

    Maternal transfer of elevated selenium (Se) to offspring is an important route of Se exposure for fish in the natural environment. However, there is a lack of information on the tissue specific spatial distribution and speciation of Se in the early developmental stages of fish, which provide important information about Se toxicokinetics. The effect of maternal transfer of Se was studied by feeding adult zebrafish a Se-elevated or a control diet followed by collection of larvae from both groups. Novel confocal synchrotron-based techniques were used to investigate Se within intact preserved larvae. Confocal X-ray fluorescence imaging was used to compare Se distributions within specific planes of an intact larva from each of the two groups. The elevated Se treatment showed substantially higher Se levels than the control; Se preferentially accumulated to highest levels in the eye lens, with lower levels in the retina, yolk and other tissues. Confocal X-ray absorption spectroscopy was used to determine that the speciation of Se within the eye lens of the intact larva was a selenomethionine-like species. Preferential accumulation of Se in the eye lens may suggest a direct cause-and-effect relationship between exposure to elevated Se and Se-induced ocular impairments reported previously. This study illustrates the effectiveness of confocal X-ray fluorescence methods for investigating trace element distribution and speciation in intact biological specimens

  14. A borax fusion technique for quantitative X-ray fluorescence analysis

    NARCIS (Netherlands)

    Willigen, van J.H.H.G.; Kruidhof, H.; Dahmen, E.A.M.F.

    1971-01-01

    A borax fusion technique to cast glass discs for quantitative X-ray analysis is described in detail. The method is based on the “nonwetting” properties of a Pt/Au alloy towards molten borax, on the favourable composition of the flux and finally on the favourable form of the casting mould. The critic

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

    CERN Document Server

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

    2002-01-01

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

  16. Synchrotron X-ray fluorescence microscopy of gallium in bladder tissue following gallium maltolate administration during urinary tract infection.

    Science.gov (United States)

    Ball, Katherine R; Sampieri, Francesca; Chirino, Manuel; Hamilton, Don L; Blyth, Robert I R; Sham, Tsun-Kong; Dowling, Patricia M; Thompson, Julie

    2013-11-01

    A mouse model of cystitis caused by uropathogenic Escherichia coli was used to study the distribution of gallium in bladder tissue following oral administration of gallium maltolate during urinary tract infection. The median concentration of gallium in homogenized bladder tissue from infected mice was 1.93 μg/g after daily administration of gallium maltolate for 5 days. Synchrotron X-ray fluorescence imaging and X-ray absorption spectroscopy of bladder sections confirmed that gallium arrived at the transitional epithelium, a potential site of uropathogenic E. coli infection. Gallium and iron were similarly but not identically distributed in the tissues, suggesting that at least some distribution mechanisms are not common between the two elements. The results of this study indicate that gallium maltolate may be a suitable candidate for further development as a novel antimicrobial therapy for urinary tract infections caused by uropathogenic E. coli.

  17. Investigation of defect luminescence from multicrystalline Si wafer solar cells using X-ray fluorescence and luminescence imaging

    Energy Technology Data Exchange (ETDEWEB)

    Peloso, Matthew P. [Department of Electrical and Computer Engineering, National University of Singapore (Singapore); Palina, Natalie; Hidayat, Hidayat; Hoex, Bram [Solar Energy Research Institute of Singapore (SERIS), National University of Singapore (Singapore); Banas, Krzysztof; Banas, Agnieszka; Breese, Mark B.H. [Singapore Synchrotron Light Source, National University of Singapore (Singapore); Aberle, Armin G. [Department of Electrical and Computer Engineering, National University of Singapore (Singapore); Solar Energy Research Institute of Singapore (SERIS), National University of Singapore (Singapore)

    2012-12-15

    Multicrystalline silicon wafer solar cells reveal performance- reducing defects by luminescence. X-ray fluorescence spectra are used to investigate the elemental constituents from regions of solar cells yielding reverse-bias or sub-bandgap luminescence from defects. It is found that a higher concentration of metals is present in regions yielding reverse-bias electroluminescence than in regions yielding sub-bandgap electroluminescence. This suggests, dislocations do not create strong breakdown currents in the absence of impurity precipitates. (a) Topographies of sub-bandgap (red) and reverse-bias (blue) luminescence from defects in a multicrystalline Si wafer solar cell. (b) Their distinct X-ray spectra indicate highest concentrations of metals in the blue regions. (copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  18. Optimizing the Elemental Sensitivity and Focal Spot Size of a Monolithic Polycapillary Optic Using Micro-X-Ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Worley, C.; Havrilla, G.; Gao, N.; Xia, Q.-F.

    1998-10-01

    A commercial micro-X-ray fluorescence (MXRF) instrument with an aperture X-ray guide was used to compare elemental sensitivities and focal spot sizes with those obtained by focusing the source with a monolithic polycapillary optic retrofitted into the system. The capillary provided an intensity gain of 125 at 4 keV vs. using a pinhole beam collimator; however, this gain advantage declined with increasing analyte line energy as a result of the capillary being designed shorter than its optimal length to fit into the commercial instrument. A minimum capillary focal spot FWHM of 36 {micro}m was achieved, whereas the smallest pinhole aperture available of 50 {micro}m in diameter produced a focal spot width of 69 {micro}m FWHM. Hence, better MXRF lateral resolution could be obtained with the capillary with a simultaneous improvement in elemental sensitivity.

  19. Synchrotron X-Ray Fluorescence Microscopy of Gallium in Bladder Tissue following Gallium Maltolate Administration during Urinary Tract Infection

    Science.gov (United States)

    Sampieri, Francesca; Chirino, Manuel; Hamilton, Don L.; Blyth, Robert I. R.; Sham, Tsun-Kong; Dowling, Patricia M.; Thompson, Julie

    2013-01-01

    A mouse model of cystitis caused by uropathogenic Escherichia coli was used to study the distribution of gallium in bladder tissue following oral administration of gallium maltolate during urinary tract infection. The median concentration of gallium in homogenized bladder tissue from infected mice was 1.93 μg/g after daily administration of gallium maltolate for 5 days. Synchrotron X-ray fluorescence imaging and X-ray absorption spectroscopy of bladder sections confirmed that gallium arrived at the transitional epithelium, a potential site of uropathogenic E. coli infection. Gallium and iron were similarly but not identically distributed in the tissues, suggesting that at least some distribution mechanisms are not common between the two elements. The results of this study indicate that gallium maltolate may be a suitable candidate for further development as a novel antimicrobial therapy for urinary tract infections caused by uropathogenic E. coli. PMID:23877680

  20. Automation of 3D micro object handling process

    DEFF Research Database (Denmark)

    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 ...

  1. Angular dependence of Ll, L $\\alpha$ , L $\\beta$ and L $\\gamma$ X-ray differential and fluorescence cross-sections for Er, Ta, W, Au, Hg and Tl

    CERN Document Server

    Demir, L; Kurucu, Y; Karabulut, A; Sahin, Y; 10.1016/S0969-806X(02)00501-7

    2003-01-01

    Ll, L alpha , L beta and L gamma X-ray differential cross-sections, fluorescence cross-sections and L/sub i/-subshell ( sigma /sub L1/, sigma /sub L2/, and sigma /sub L3/) fluorescence cross-sections were measured for Er, Ta, W, Au, Hg, and Tl at an excitation energy of 59.6 keV using a Si(Li) detector. The differential cross-sections for these elements have been measured at different angles varying from 54 degrees to 153 degrees at intervals of 9 degrees . The Ll and L alpha groups in the L X-ray lines are found to be spatially anisotropic, while those in the L beta and L gamma peaks are isotropic. Experimental and theoretical values of L X-ray fluorescence cross- sections and L/sub i/-subshell X-ray fluorescence cross-sections were compared. (20 refs).

  2. Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear (LIN)]. E-mail: edualm@usp.br; Leite, Laudi C.; Lanna, Dante P.D. [Escola Superior de Agricultura ' Luiz de Queiroz' (ESALQ/USP), Piracicaba, SP (Brazil). Dept. de Zootecnia. Lab. de Anatomia e Fisiologia Animal (LAFA)]. E-mail: lcleite@ciagri.usp.br

    2007-07-01

    The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 {mu}L of the sample were dried at 60 deg C on 6.35 {mu}m Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

  3. Cr and Yb markers determination in animal feces by energy dispersive X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Eduardo de; Senicato, Luis A; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear (LIN)]. E-mail: edualm@usp.br; Gomide, Catarina A. [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil). Faculdade de Zootecnia e Engenharia de Alimentos (FZEA). Dept. de Zootecnia]. E-mail: cbgomide@usp.br

    2007-07-01

    Chromium and Ytterbium elements are utilized in animal nutritional studies as markers. This paper describes an analytical method for Cr and Yb determination in solid buffalo feces sample using standard addition method and energy dispersive X-ray spectrometry (EDXRF) technique. One gram dried sample was pressed manually in an XRF sample cup with Mylar film (6.3 {mu}m thickness) in the bottom. The experimental conditions were: Mo target X-ray tube with Zr filter, operated at 25 kV/10 mA, and 500 s of acquisition time. The limits of detection for Cr and Yb were 16.6 and 11.4 mg/kg, respectively. This methodology has showed appropriated for simultaneous Cr and Yb determination as marker in animal feces. (author)

  4. Possible Radiation-Induced Damage to the Molecular Structure of Wooden Artifacts Due to Micro-Computed Tomography, Handheld X-Ray Fluorescence, and X-Ray Photoelectron Spectroscopic Techniques

    Directory of Open Access Journals (Sweden)

    Madalena Kozachuk

    2016-05-01

    Full Text Available This study was undertaken to ascertain whether radiation produced by X-ray photoelectron spectroscopy (XPS, micro-computed tomography (μCT and/or portable handheld X-ray fluorescence (XRF equipment might damage wood artifacts during analysis. Changes at the molecular level were monitored by Fourier transform infrared (FTIR analysis. No significant changes in FTIR spectra were observed as a result of μCT or handheld XRF analysis. No substantial changes in the collected FTIR spectra were observed when XPS analytical times on the order of minutes were used. However, XPS analysis collected over tens of hours did produce significant changes in the FTIR spectra.

  5. Laboratory Tests of a Handheld X-Ray Fluorescence Spectrometer: A Tool for Planetary Exploration

    Science.gov (United States)

    Young, K. E.; Evans, C. A.; Hodges, K.

    2011-12-01

    Maximizing the science return from a mission to another planetary surface involves the integration of science objectives with deployable technologies that enable the collection of data and samples. For long duration manned missions, it is likely that more samples will be collected than can be returned to Earth due to mass limits. A niche exists for technologies that help prioritize samples for return, provide data for future sample handling and curation, and characterization for samples that are not returned to Earth. To fill this niche, hardware and protocols for field instruments are currently being developed and evaluated at NASA Johnson Space Center and Arizona State University. Our goal is to develop an easily used, environmentally isolated facility as part of the astronaut surface habitat for preliminary sample characterization and down-selection. NASA has constructed a prototype, GeoLab, as a testbed for evaluating the scientific applicability and operational considerations of various analytical instruments. One instrument under evaluation is a small, portable x-ray fluorescence (XRF) spectrometer that can be also be used by astronaut explorers as part of their field gear while on scientific sorties, or on robotic field assistants. We report on preliminary usability tests for commercially available handheld XRF instruments. These instruments collect data by contacting the surface of a rock or sediment sample with an 8 mm-wide sensor window. Within 60 seconds, the devices can provide relatively precise data on the abundance of major and trace elements heavier than Na. Lab-based handheld XRF analyses of terrestrial and lunar samples, compared with those made with full-scale laboratory XRF systems, show good correlation, but we continue to investigate potential sources of error and the need for careful calibration with standards of known composition. Specifically, we use a suite of five terrestrial and five lunar basalts, all well characterized by conventional

  6. Pigments Elementary Chemical Composition Study of a Gainsborough Attributed Painting Employing a Portable X-Rays Fluorescence System

    Science.gov (United States)

    Appoloni, C. R.; Blonski, M. S.; Parreira, P. S.; Souza, L. A. C.

    2007-02-01

    The investigated painting, identified with the title "The woodman", is attributed to Thomas Gainsborough (XVIII century) and is under investigation at the Laboratory of Conservation Science (LACICOR), CECOR/EBA/UFMG. The measurements were carried out with a portable X-rays fluorescence (XRF) system constituted of a X-rays tube with Ag anode, a Si PIN — diode detector, nuclear electronic chain and a special designed mechanical system for the detector and X-ray tube positioning, that enables angular and XYZ movements of the excitation-detection system. The employed voltage and current intensity were 17 kV and 3 mA, respectively. The time of acquisition for each measurement was 500 s. XRF spectra were analyzed using the AXIL-WinQXAS software. Three measurements in each of the following regions of the painting were done: face, leaves, arm, sky and firewood. The carried out analysis indicated the following pigments: White (lead white and calcium sulfate, identified by the elements Pb, Ca and S), Blue (Prussian blue, identified by the key element Fe), Red (Vermilion, identified by the elements Hg and S) and Brown (mixture of Fe and Mn oxides, identified by the elements Fe and Mn). Elements belonging to modern pigments corresponding to the same colors were absent in the analyzed spectra.

  7. The surface morphology analysis based on progressive approximation method using confocal three-dimensional micro X-ray fluorescence

    Science.gov (United States)

    Yi, Longtao; Sun, Tianxi; Wang, Kai; Qin, Min; Yang, Kui; Wang, Jinbang; Liu, Zhiguo

    2016-08-01

    Confocal three-dimensional micro X-ray fluorescence (3D MXRF) is an excellent surface analysis technology. For a confocal structure, only the X-rays from the confocal volume can be detected. Confocal 3D MXRF has been widely used for analysing elements, the distribution of elements and 3D image of some special samples. However, it has rarely been applied to analysing surface topography by surface scanning. In this paper, a confocal 3D MXRF technology based on polycapillary X-ray optics was proposed for determining surface topography. A corresponding surface adaptive algorithm based on a progressive approximation method was designed to obtain surface topography. The surface topography of the letter "R" on a coin of the People's Republic of China and a small pit on painted pottery were obtained. The surface topography of the "R" and the pit are clearly shown in the two figures. Compared with the method in our previous study, it exhibits a higher scanning efficiency. This approach could be used for two-dimensional (2D) elemental mapping or 3D elemental voxel mapping measurements as an auxiliary method. It also could be used for analysing elemental mapping while obtaining the surface topography of a sample in 2D elemental mapping measurement.

  8. Fluorescence-based knife-edge beam diameter measurement to characterize X-ray beam profiles in reflection geometry

    Science.gov (United States)

    Bassel, Léna; Tauzin, Xavier; Queffelec, Alain; Ferrier, Catherine; Lacanette, Delphine; Chapoulie, Rémy; Bousquet, Bruno

    2016-04-01

    The diameter of an X-ray beam was determined, using the knife-edge technique, widely applied for beam profiling, by taking advantage of the fluorescence emission generated by the X-ray beam. The knife-edge has to be appropriate to the configuration of the device, in our case a double-material target made of plastic and cardboard was scanned in a transversal plane compared to the beam propagation direction. Along the scanning axis, for each position, the intensity of the Kα line of chlorine was recorded. The first derivative of the intensity evolution as a function of the edge position, fitted by a Gaussian function, makes it possible to obtain the beam diameter along the scan direction. We measured a slightly elliptic diameter close to 3 mm. In this note we underline the significance of the knife-edge technique which represents a useful tool, easy to be set up, to control X-ray beam dimensions in portable devices often routinely used by non-specialists.

  9. Evaluation of the composition of filters additional of equipment radiological intraoral by energy dispersive x-ray fluorescence (EDXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Franca, Alana Caroline; Torres, Catarina A.M.P.; Rocha, Ana S.S.; Deniak, Valeriy; Lara, Alessandro L.; Paschuk, Sergei A., E-mail: alanacarolinef@gmail.com, E-mail: sergei@utfpr.edu.br [Universidade Tecnologica Federal do Parana (CPGEI/UTFPR), Curitiba, PR (Brazil). Programa de Pos-Graduacao em Engenharia Eletrica e Informatica Industrial; Fernandes, Angela; Westphalen, Fernando Henrique, E-mail: angelafernandes@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Setor de Ciencias da Saude

    2013-07-01

    The need for high quality standards for radiographic images in order to make a diagnosis assertive, and being the additional filtration required in the intraoral X-ray equipment show the need of evaluating these filters. This study aims to examine the influence of the elemental composition of the filters of X-ray of dental intraoral equipment in the radiographic images quality. The filters analysis were performed by using the energy dispersive X-ray fluorescence method (EDXRF). Ten conventional filters were analysed. In this study, 33 radiographic exposures were performed using films: twenty radiographs in the incisor region and ten in the molar region, three exposures were also made in the same regions with same conditions without using filter. After radiographs development, optical density was measure and all radiographs were submitted to subjective evaluation by dental radiologists. Data obtained were correlated to effects evaluation of the elemental composition of all filters in the quality of the radiographic images. The elements found were: aluminum, cobalt, copper, sulfur, iron, manganese, titanium, zinc, and zirconium. The images obtained were identified in groups: Molars to 0.3 s; Incisors to 0.2 s; Incisors to 0.3 s, and for the group without filters. From the results obtained it was concluded that both unclear radiographs and ideal radiographs were produced by using filters of elementary common. Therefore, conventional filters evaluated were an acceptable option to produce quality images in dental radiology, despite differences in the composition of the alloys. (author)

  10. Engineering iodine-doped carbon dots as dual-modal probes for fluorescence and X-ray CT imaging.

    Science.gov (United States)

    Zhang, Miaomiao; Ju, Huixiang; Zhang, Li; Sun, Mingzhong; Zhou, Zhongwei; Dai, Zhenyu; Zhang, Lirong; Gong, Aihua; Wu, Chaoyao; Du, Fengyi

    2015-01-01

    X-ray computed tomography (CT) is the most commonly used imaging technique for noninvasive diagnosis of disease. In order to improve tissue specificity and prevent adverse effects, we report the design and synthesis of iodine-doped carbon dots (I-doped CDs) as efficient CT contrast agents and fluorescence probe by a facile bottom-up hydrothermal carbonization process. The as-prepared I-doped CDs are monodispersed spherical nanoparticles (a diameter of ~2.7 nm) with favorable dispersibility and colloidal stability in water. The aqueous solution of I-doped CDs showed wavelength-dependent excitation and stable photoluminescence similar to traditional carbon quantum dots. Importantly, I-doped CDs displayed superior X-ray attenuation properties in vitro and excellent biocompatibility. After intravenous injection, I-doped CDs were distributed throughout the body and excreted by renal clearance. These findings validated that I-doped CDs with high X-ray attenuation potency and favorable photoluminescence show great promise for biomedical research and disease diagnosis.

  11. A high-quality multilayer structure characterization method based on X-ray fluorescence and Monte Carlo simulation

    Energy Technology Data Exchange (ETDEWEB)

    Brunetti, Antonio; Golosio, Bruno [Universita degli Studi di Sassari, Dipartimento di Scienze Politiche, Scienze della Comunicazione e Ingegneria dell' Informazione, Sassari (Italy); Melis, Maria Grazia [Universita degli Studi di Sassari, Dipartimento di Storia, Scienze dell' Uomo e della Formazione, Sassari (Italy); Mura, Stefania [Universita degli Studi di Sassari, Dipartimento di Agraria e Nucleo di Ricerca sulla Desertificazione, Sassari (Italy)

    2014-11-08

    X-ray fluorescence (XRF) is a well known nondestructive technique. It is also applied to multilayer characterization, due to its possibility of estimating both composition and thickness of the layers. Several kinds of cultural heritage samples can be considered as a complex multilayer, such as paintings or decorated objects or some types of metallic samples. Furthermore, they often have rough surfaces and this makes a precise determination of the structure and composition harder. The standard quantitative XRF approach does not take into account this aspect. In this paper, we propose a novel approach based on a combined use of X-ray measurements performed with a polychromatic beam and Monte Carlo simulations. All the information contained in an X-ray spectrum is used. This approach allows obtaining a very good estimation of the sample contents both in terms of chemical elements and material thickness, and in this sense, represents an improvement of the possibility of XRF measurements. Some examples will be examined and discussed. (orig.)

  12. Calibration of handheld X-ray fluorescence (XRF) equipment for optimum determination of elemental concentrations in sediment samples.

    Science.gov (United States)

    Mejía-Piña, K Gabriela; Huerta-Diaz, Miguel Angel; González-Yajimovich, O

    2016-12-01

    Handheld X-ray fluorescence spectrometers (XRFs) represent a more practical, efficient and economic tool to determine the elemental composition of solid inorganic and organic samples than conventional analytical techniques. The objective of this work was to demonstrate that handheld XRFs could be a precise, accurate and reliable tool to analyze up to 27 different elements. This objective was accomplished through the optimization of an empirical calibration curve that, in addition to include certified reference materials (CRM), it also introduced new approaches, such as the use of solid CRM mixtures and combinations of organic and inorganic matrices. These approaches significantly increased the number of calibration points and eliminated hiatuses in the calibration curve. Several factors were evaluated before construction of the calibration curve: incidence time of the X-ray beam, type of film through which the X-ray beams reach the samples, container type, minimum sample volume and sample moisture content. Results show that single elements can be analyzed with variable exposure times or, alternatively, multielemental analyses can be carried out with a constant exposure time (180s). Costs can be reduced by using Ziploc(®) bags as sample containers, but the number of measurable elements drops from 27 to 21, while the possibility of contamination increases.

  13. The study of in vivo x-ray fluorescence (XRF) technique for gadolinium (Gd) measurements in human bone

    Science.gov (United States)

    Mostafaei, F.; Nie, L. H.

    2016-08-01

    An in vivo K x-ray fluorescence system, based on 109Cd source, for the detection of gadolinium has been investigated. Gd is of interest because of the extensive use of Gd-based contrast agents in MR imaging. A human simulating bone phantom set has been developed. The phantoms were doped with seven concentrations of Gd. Additional elements important for in vivo x-ray fluorescence, Na, Cl and Ca, were also included to create an overall elemental composition consistent with the Reference Man. A new 5 GBq 109Cd source was purchased to improve the source activity in comparison to the previous study (0.17 GBq). The previously published minimum detection limit (MDL) for Gd phantom measurements using KXRF system was 3.3 ppm. In this study the minimum detection limit for bare bone phantoms was found to reduce the MDL to 0.8, a factor of 4.1. The previous published data used only three layers of plastic as soft tissue equivalent materials and found the MDL of 4-4.8 ppm. In this study we have used the plastic with more realistic thicknesses to simulate a soft tissue at tibia. The detection limits for phantoms with Lucite as a tissue equivalent, using a new source, was determined to be 1.81 to 3.47 ppm (μg Gd per gram phantom). Our next study would be testing an in vivo K x-ray fluorescence system, based on 109Cd source on human volunteers who went through MR imaging and were injected by Gd.

  14. Germanium Collimating micro-Channel Arrays For High Resolution, High Energy Confocal X-ray Fluorescence Microscopy

    CERN Document Server

    Agyeman-Budu, David N; Coulthard, Ian; Gordon, Robert; Hallin, Emil; Woll, Arthur R

    2016-01-01

    Confocal x-ray fluorescence microscopy (CXRF) allows direct detection of x-ray fluorescence from a micron-scale 3D volume of an extended, unthinned sample. We have previously demonstrated the use of a novel collection optic, fabricated from silicon, that improves the spatial resolution of this approach by an order of magnitude over CXRF using polycapillaries. The optic, called a collimating channel array (CCA), consists of micron-scale, lithographically-fabricated arrays of collimating channels, all directed towards a single source position. Due to the limited absorbing power of silicon, the useful energy range of these optics was limited to fluorescence emission below about 10 keV. Here, we report fabrication of CCAs from germanium substrates, and demonstrate their practical use for CXRF up to 20 keV. Specifically we demonstrate a nearly energy-independent critical spatial resolution $d_R$ of 2.1$\\pm$0.17 \\um from 2-20 keV, as well as excellent background reduction compared to silicon-based CCAs throughout t...

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

    Science.gov (United States)

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

    2017-04-01

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

  16. Nondestructive, energy-dispersive, x-ray fluorescence analysis of actinide stream concentrations from reprocessed nuclear fuels

    Energy Technology Data Exchange (ETDEWEB)

    Camp, D.C.; Ruhter, W.D.

    1979-06-27

    In one plan for reprocessing LWR spent fuel, after separation from fission products and transplutonics, part of the U and all of the Pu in a nitrate solution will form a coprocessed stream which is then evaporated and sent to a hold tank for accounting. The remaining U fraction will be purified and sent to a separate storage tank. These two streams can be monitored using x-ray fluorescence analysis. This report discusses equipment, spectra, cell calibration, and dynamic concentration measurements. 7 figures. (DLC)

  17. In situ analysis of trace elements in metalloproteins of human liver by synchrotron radiation X-ray fluorescence

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A method using synchrotron radiation X-ray fluorescence analysis to in situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands for human liver cytosolic sample separated by SDS-PAGE was analyzed along polyacrylamide gel. The results showed that the protein fraction of peak III in cytosol was mainly composed of metal ion Zn-associated proteins, being in agreement with that given by atomic absorption spectrometry. Thus, it demonstrated the feasibility of this novel technique for in situ analysis of trace elements in protein bands.

  18. In situ analysis of trace elements in metalloproteins of human liver by synchrotron radiation X-ray fluorescence

    Institute of Scientific and Technical Information of China (English)

    陈春英; 章佩群; 柴之芳; 李光城; 黄宇营

    2000-01-01

    A method using synchrotron radiation X-ray fluorescence analysis to in situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands for human liver cytosolic sample separated by SDS-PAGE was analyzed a-long polyacrylamide gel. The results showed that the protein fraction of peak III in cvtosol was mainly composed of metal ion Zn-associated proteins, being in agreement with that given by atomic absorption spectrometry. Thus, it demonstrated the feasibility of this novel technique for in situ analysis of trace elements in protein bands.

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

    Energy Technology Data Exchange (ETDEWEB)

    Soares, Julio C.A.C.R.; Canellas, Catarine G.L.; Lopes, Ricardo T., E-mail: ricardo@lin.ufrj.br, E-mail: jcorsini@lin.ufrj.br [Nuclear Laboratory Instrumentation/COPPE, Federal University of Rio de Janeiro (UFRJ), Rio de Janeiro, RJ (Brazil); Anjos, Marcelino J., E-mail: marcelin@lin.ufrj.br [Physics Institute, State University of Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil)

    2011-07-01

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

  20. Elemental concentrations in skin of patients with fibroeptelial polip using synchrotron radiation total reflection x-ray fluorescence

    Science.gov (United States)

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

    2012-05-01

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

  1. Use of portable X-ray fluorescence spectrometry for environmental quality assessment of peri-urban agriculture.

    Science.gov (United States)

    Weindorf, David C; Zhu, Yuanda; Chakraborty, Somsubhra; Bakr, Noura; Huang, Biao

    2012-01-01

    Urban expansion into traditional agricultural lands has augmented the potential for heavy metal contamination of soils. This study examined the utility of field portable X-ray fluorescence (PXRF) spectrometry for evaluating the environmental quality of sugarcane fields near two industrial complexes in Louisiana, USA. Results indicated that PXRF provided quality results of heavy metal levels comparable to traditional laboratory analysis. When coupled with global positioning system technology, the use of PXRF allows for on-site interpolation of heavy metal levels in a matter of minutes. Field portable XRF was shown to be an effective tool for rapid assessment of heavy metals in soils of peri-urban agricultural areas.

  2. The study of chemical composition and elemental mappings of colored over-glaze porcelain fired in Qing Dynasty by micro-X-ray fluorescence

    Science.gov (United States)

    Lin, Cheng; Meitian, Li; Youshi, Kim; Changsheng, Fan; Shanghai, Wang; Qiuli, Pan; Zhiguo, Liu; Rongwu, Li

    2011-02-01

    It is very difficult to measure the chemical composition of colored pigments of over-glaze porcelain by X-ray fluorescence because it contains high concentration of Pb. One of the disadvantages of our polycapillary optics is that it has low transmission efficiency to the high energy X-ray. However, it is beneficial to measure the chemical compositions of rich Pb sample. In this paper, we reported the performances of a tabletop setup of micro-X-ray fluorescence system base on slightly focusing polycapillary and its applications for analysis of rich Pb sample. A piece of Chinese ancient over-glaze porcelain was analyzed by micro-X-ray fluorescence. The experimental results showed that the Cu, Fe and Mn are the major color elements. The possibilities of the process of decorative technology were discussed in this paper, also.

  3. [Determinations of silicon and phosphorus in rice planted in a district of high incidence of amyotrophic lateral sclerosis by neutron activation and X-ray fluorescence analyses].

    Science.gov (United States)

    Mizumoto, Y; Ishikawa, T; Kusakabe, T; Katsurayama, K; Iwata, S

    1989-12-01

    Silicon and phosphorus contents in polished and unpolished rice planted in a district of high incidence of amyotrophic lateral sclerosis (ALS) have been determined by neutron activation and X-ray fluorescence methods, and compared with those from control areas. In the neutron activation analysis, beta-ray spectra of 32P produced by the 31P(n, gamma)32P reaction on polished and unpolished rice were measured with a low background beta-ray spectrometer. In the X-ray fluorescence analysis, characteristic X-rays were analyzed with a wavelength dispersive X-ray fluorescence spectrometer. Silicon contents in polished and unpolished rice from the ALS area are 42 micrograms.g-1 and 370 micrograms.g-1, respectively, and the corresponding phosphorus contents are 1,210 micrograms.g-1, and 3,370 micrograms.g-1, respectively. The data for ALS area are equal to those for the control area within standard deviation.

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

    Science.gov (United States)

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

    2010-06-01

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

  5. Mapping alpha-Particle X-Ray Fluorescence Spectrometer (Map-X)

    Science.gov (United States)

    Blake, D. F.; Sarrazin, P.; Bristow, T.

    2014-01-01

    Many planetary surface processes (like physical and chemical weathering, water activity, diagenesis, low-temperature or impact metamorphism, and biogenic activity) leave traces of their actions as features in the size range 10s to 100s of micron. The Mapping alpha-particle X-ray Spectrometer ("Map-X") is intended to provide chemical imaging at 2 orders of magnitude higher spatial resolution than previously flown instruments, yielding elemental chemistry at or below the scale length where many relict physical, chemical, and biological features can be imaged and interpreted in ancient rocks.

  6. A bench-top K X-ray fluorescence system for quantitative measurement of gold nanoparticles for biological sample diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Ricketts, K., E-mail: k.ricketts@ucl.ac.uk [Division of Surgery and Interventional Sciences, University College London, Royal Free Campus, Rowland Hill Street, London NW3 2PF (United Kingdom); Guazzoni, C.; Castoldi, A. [Dipartimento di Elettronica, Informazione e Bioingegneria Politecnico di Milano and INFN, Sezione di Milano P.za Leonardo da Vinci, 32-20133 Milano (Italy); Royle, G. [Department of Medical Physics and Bioengineering, University College London, Malet Place Engineering Building, Gower Street, London WC1E 6BT (United Kingdom)

    2016-04-21

    Gold nanoparticles can be targeted to biomarkers to give functional information on a range of tumour characteristics. X-ray fluorescence (XRF) techniques offer potential quantitative measurement of the distribution of such heavy metal nanoparticles. Biologists are developing 3D tissue engineered cellular models on the centimetre scale to optimise targeting techniques of nanoparticles to a range of tumour characteristics. Here we present a high energy bench-top K-X-ray fluorescence system designed for sensitivity to bulk measurement of gold nanoparticle concentration for intended use in such thick biological samples. Previous work has demonstrated use of a L-XRF system in measuring gold concentrations but being a low energy technique it is restricted to thin samples or superficial tumours. The presented system comprised a high purity germanium detector and filtered tungsten X-ray source, capable of quantitative measurement of gold nanoparticle concentration of thicker samples. The developed system achieved a measured detection limit of between 0.2 and 0.6 mgAu/ml, meeting specifications of biologists and being approximately one order of magnitude better than the detection limit of alternative K-XRF nanoparticle detection techniques. The scatter-corrected K-XRF signal of gold was linear with GNP concentrations down to the detection limit, thus demonstrating potential in GNP concentration quantification. The K-XRF system demonstrated between 5 and 9 times less sensitivity than a previous L-XRF bench-top system, due to a fundamental limitation of lower photoelectric interaction probabilities at higher K-edge energies. Importantly, the K-XRF technique is however less affected by overlying thickness, and so offers future potential in interrogating thick biological samples.

  7. X-ray fluorescence study of the concentration of selected trace and minor elements in human brain tumours

    Science.gov (United States)

    Wandzilak, Aleksandra; Czyzycki, Mateusz; Radwanska, Edyta; Adamek, Dariusz; Geraki, Kalotina; Lankosz, Marek

    2015-12-01

    Neoplastic and healthy brain tissues were analysed to discern the changes in the spatial distribution and overall concentration of elements using micro X-ray fluorescence spectroscopy. High-resolution distribution maps of minor and trace elements such as P, S, Cl, K, Ca, Fe, Cu and Zn made it possible to distinguish between homogeneous cancerous tissue and areas where some structures could be identified, such as blood vessels and calcifications. Concentrations of the elements in the selected homogeneous areas of brain tissue were compared between tumours with various malignancy grades and with the controls. The study showed a decrease in the average concentration of Fe, P, S and Ca in tissues with high grades of malignancy as compared to the control group, whereas the concentration of Zn in these tissues was increased. The changes in the concentration were found to be correlated with the tumour malignancy grade. The efficacy of micro X-ray fluorescence spectroscopy to distinguish between various types of cancer based on the concentrations of studied elements was confirmed by multivariate discriminant analysis. Our analysis showed that the most important elements for tissue classification are Cu, K, Fe, Ca, and Zn. This method made it possible to correctly classify histopathological types in 99.93% of the cases used to build the model and in as much as 99.16% of new cases.

  8. On-line monitoring of particulate iron oxides in steam generator feedwater using x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Stauffer, C.C.; Connolly, D.J. [Babcock and Wilcox, Alliance, OH (United States). Research and Development Division; Millett, P.J. [Electric Power Research Inst., Palo Alto, CA (United States)

    1995-12-01

    Corrosion product monitoring is important as power plants strive to minimize corrosion and maximize availability. Current methodology for monitoring corrosion products involves grab sampling and/or collection of integrated samples using membrane filters followed by analysis of the membranes in the laboratory. This technique is labor intensive and provides only average values over lengthy sampling intervals (typically 1--3 days). Recently, a laboratory tool -- x-ray fluorescence (XRF) spectroscopy -- was combined with existing on-line sampling techniques resulting in an on-line XRF monitor capable of measuring iron oxide particulates in a flowing stream at the parts-per-billion (ppb) level and below. After development in the laboratory, the instrument was successfully field tested in two power plants. After testing at the first power plant, modifications to improve instrument performance were incorporated. This paper presents information regarding design and operation of the instrument, improvements made during the first test period, and field data obtained during plant service. Results show that this instrument will provide on-line measurements of iron oxides at the ppb level with minimal operator involvement. Finally, there are wider applications for this on-line XRF monitor. Though the present system is geared toward iron analysis in corrosion products, it could as well be configured for other elements or groups of elements for other applications such lead, sulfur, copper, chromium, or any other element detectable by x-ray fluorescence.

  9. Analytical possibilities of different X-ray fluorescence systems for determination of trace elements in aqueous samples pre-concentrated with carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Marguí, E., E-mail: eva.margui@udg.edu [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain); Zawisza, B.; Skorek, R. [Institute of Chemistry, University of Silesia, Szkolna 9, 40-006 Katowice (Poland); Theato, T. [SPECTRO Analytical Instruments GmbH, Boschstr. 10, 47533 Kleve (Germany); Queralt, I. [Laboratory of X-Ray Analytical Applications, Institute of Earth Sciences Jaume Almera, CSIC, Solé Sabarís s/n, 08028 Barcelona (Spain); Hidalgo, M. [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain); Sitko, R. [Institute of Chemistry, University of Silesia, Szkolna 9, 40-006 Katowice (Poland)

    2013-10-01

    This study was aimed to achieve improved instrumental sensitivity and detection limits for multielement determination of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Pb and Cd in liquid samples by using different X-ray fluorescence (XRF) configurations (a benchtop energy-dispersive X-ray fluorescence spectrometer, a benchtop polarised energy-dispersive X-ray fluorescence spectrometer and a wavelength-dispersive X-ray fluorescence spectrometer). The preconcentration of metals from liquid solutions consisted on a solid-phase extraction using carbon nanotubes (CNTs) as solid sorbents. After the extraction step, the aqueous sample was filtered and CNTs with the absorbed elements were collected onto a filter paper which was directly analyzed by XRF. The calculated detection limits in all cases were in the low ng mL{sup −1} range. Nevertheless, results obtained indicate the benefits, in terms of sensitivity, of using polarized X-ray sources using different secondary targets in comparison to conventional XRF systems, above all if Cd determination is required. The developed methodologies, using the aforementioned equipments, have been applied for multielement determination in water samples from an industrial area of Poland. - Highlights: • Use of carbon nanotubes for preconcentration of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Pb and Cd • Combination of this preconcentration procedure with different XRF systems • Benefit of using polarized X-ray sources for trace element determination.

  10. Development of a portable system of X-ray fluorescence spectrometry; Desenvolvimento de um sistema portatil de espectrometria por fluorescencia de raios X

    Energy Technology Data Exchange (ETDEWEB)

    Mantuano, Andrea; Crisostomo, Jose V.V.; Barros, Mariana J.; Oliveira, Luis F.; Barroso, Regina C., E-mail: andreafisica@yahoo.com.b, E-mail: jose_vicente_crisostomo@yahoo.com.b, E-mail: mariana_jbarros@yahoo.co, E-mail: lfolive@oi.com.b, E-mail: cely_barroso@hotmail.co [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Inst. de Fisica

    2009-07-01

    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

  11. Simple procedure for nutrient analysis of coffee plant with energy dispersive X-ray fluorescence spectrometry (EDXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Tezotto, Tiago; Favarin, Jose Laercio; Neto, Ana Paula; Azevedo, Ricardo Antunes, E-mail: tiago.tezotto@usp.br [Escola Superior de Agricultura Luiz de Queiroz (ESALQ/USP), Piracicaba, SP (Brazil); Gratao, Priscila Lupino [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP/ FCAV), Jaboticabal, SP (Brazil). Dept. de Biologia Aplicada a Agropecuaria; Mazzafera, Paulo [Universidade Estadual de Campinas (UNICAMP/IB), SP (Brazil). Dept. Biologia Vegetal

    2013-07-15

    Nutrient analysis is used to estimate nutrient content of crop plants to manage fertilizer application for sustained crop production. Direct solid analysis of agricultural and environmental samples by energy dispersive X-ray fluorescence spectrometry (EDXRF) was chosen as alternative technique to evaluate the simultaneous multielemental quantification of the most important essential elements in coffee (Coffea arabica L.) plants. Inductively coupled plasma atomic emission spectrometry and certified reference materials made from leaves were used to calibrate and check the trueness of EDXRF method for the determination of the concentration of several nutrients in coffee leaves and branches. Fluorescence spectrometry proved to be advantageous and presented low cost as loose powder samples could be used. Samples collected from a field experiment where coffee plants were treated with excess of Ni and Zn were used to verify the practical application of the method. Good relationships were achieved between certified values and data obtained by EDXRF, with recoveries ranging from 82 to 117 %.(author)

  12. Investigation of mineral distribution in bone by synchrotron X-ray fluorescence microscopy after tibolone therapy

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Rio de Janeiro State Univ., Nova Friburgo, RJ (Brazil). Dept. of Mechanical Engineering and Energy; Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Carvalho, A.C.B.; Henriques, H.N.; Guzman-Silva, M.A. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Lab. of Experimental Pathology; Sales, E.; Lopes, R.T. [Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Granjeiro, J.M. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Dept. of Cellular and Molecular Biology

    2011-07-01

    Tibolone is a synthetic steroid with estrogenic, androgenic, and progestagenic properties used for the prevention of postmenopausal osteoporosis and treatment of climacteric symptoms. Tibolone shows almost no action on breast and endometrium, which are target-organs for estrogens and progesterone activity. The aim of this work was to investigate the spatial distribution of calcium and zinc minerals in the femoral head of ovariectomized rat in order to evaluate the effects of the long-term administration of tibolone. For that purpose X-ray microfluorescence was used with synchrotron radiation imaging technique which was performed at Brazilian Light Synchrotron Laboratory, Campinas, SP. Minerals were not homogeneously distributed in trabecular bone areas; a higher concentration of calcium in the trabecular regions at femoral heads was found in ovariectomized and tibolone-treated rats compared to ovariectomized and control groups. (orig.)

  13. Estimation of Lead (Pb in Toys Using X-Ray Fluorescence Technology

    Directory of Open Access Journals (Sweden)

    Sandipayan Dutta

    2016-01-01

    Full Text Available Background: Lead exists extensively in the environment and it is a heavy metal, which is neurotoxic in nature which is harmful to children. In contrast to trace elements such as iron (Fe and zinc (Zn, lead has no recognized benecial effects in human body. With the economic development in India in recent years, the concentration of lead has increased in the environment and henceforth, lead pollution has become a severe problem in the country. Lead poisoning can create an immense damage and irreversible harm to foetal growth, the growth of teenagers and psychological, behavioural and cognitive development. Aim and Objectives: To estimate the lead content in the sample of toys. Material and Methods: 97 different toys were collected and coded as TS, these toys were kept in plastic lock cover which were lead proof. At rst the toys were arranged in order according to the serial number of the code (TS1 – TS97. The FP X-ray uorescence (Innov-X ray analyzer instrument was placed with the window of the analyzer on the surface of the toy vertically in such a way that there was no gap between the toy surface and the sampling window. The parts per million (ppm values of all toys were recorded. Results: Out of 97 samples tested, 22 samples were above permissible limits. The different materials demonstrate signicant correlation with the lead content in ppm. Lead is used as a stabilizer in some toys as well as children's items made from PVC plastic. Baby toys made up of plastic have higher concentration of lead. Lead can leach out of products when children handle and swallow them involuntarily.

  14. Wavelength Dispersive X-ray Fluorescence Analysis of Actinides in Dissolved Nuclear Fuels

    Energy Technology Data Exchange (ETDEWEB)

    O' Hara, David [Parallax Research, Inc., Tallahassee, FL (United States)

    2015-10-15

    There is an urgent need for an instrument that can quickly measure the concentration of Plutonium and other Actinides mixed with Uranium in liquids containing dissolved spent fuel rods. Parallax Research, Inc. proposes to develop an x-ray spectrometer capable of measuring U, Np and Pu in dissolved nuclear fuel rod material to less than 10 ppm levels to aid in material process control for these nuclear materials. Due to system noise produced by high radioactivity, previous x-ray spectrometers were not capable of low level measurements but the system Parallax proposed has no direct path for undesired radiation to get to the detector and the detector in the proposed device is well shielded from scatter and has very low dark current. In addition, the proposed spectrometer could measure these three elements simultaneously, also measuring background positions with an energy resolution of roughly 100 eV making it possible to see a small amount of Pu that would be hidden under the tail of the U peak in energy dispersive spectrometers. Another nearly identical spectrometer could be used to target Am and Cm if necessary. The proposed spectrometer needs only a tiny sample of roughly 1 micro-liter (1 mm3) and the measurement can be done with the liquid flowing in a radiation and chemical immune quartz capillary protected by a stainless steel rod making it possible to continuously monitor the liquid or to use a capillary manifold to measure other liquid streams. Unlike other methods such as mass spectroscopy where the sample must be taken to a remote facility and might take days for turn-around, the proposed measurement should take less than an hour. This spectrometer could enable near real-time measurement of U, Pu and Np in dilute dissolved spent nuclear fuel rod streams.

  15. Engineering iodine-doped carbon dots as dual-modal probes for fluorescence and X-ray CT imaging

    Directory of Open Access Journals (Sweden)

    Zhang M

    2015-11-01

    Full Text Available Miaomiao Zhang,1,* Huixiang Ju,2,* Li Zhang,1,* Mingzhong Sun,2 Zhongwei Zhou,2 Zhenyu Dai,3 Lirong Zhang,1 Aihua Gong,1 Chaoyao Wu,1 Fengyi Du1 1School of Medicine, Jiangsu University, Zhenjiang, People’s Republic of China; 2Department of Clinical Laboratory, Affiliated Yancheng Hospital, School of Medicine, Southeast University, Yancheng, Jiangsu, People’s Republic of China; 3Radiology Department, Affiliated Yancheng Hospital, School of Medicine, Southeast University, Yancheng, Jiangsu, People’s Republic of China *These authors contributed equally to this work Abstract: X-ray computed tomography (CT is the most commonly used imaging technique for noninvasive diagnosis of disease. In order to improve tissue specificity and prevent adverse effects, we report the design and synthesis of iodine-doped carbon dots (I-doped CDs as efficient CT contrast agents and fluorescence probe by a facile bottom-up hydrothermal carbonization process. The as-prepared I-doped CDs are monodispersed spherical nanoparticles (a diameter of ~2.7 nm with favorable dispersibility and colloidal stability in water. The aqueous solution of I-doped CDs showed wavelength-dependent excitation and stable photoluminescence similar to traditional carbon quantum dots. Importantly, I-doped CDs displayed superior X-ray attenuation properties in vitro and excellent biocompatibility. After intravenous injection, I-doped CDs were distributed throughout the body and excreted by renal clearance. These findings validated that I-doped CDs with high X-ray attenuation potency and favorable photoluminescence show great promise for biomedical research and disease diagnosis. Keywords: carbon dots, contrast agents, iodine-doped, CT imaging

  16. Analysis of individual fluid inclusions using synchrotron X-ray fluorescence microprobe: progress toward calibration for trace elements

    Science.gov (United States)

    Ménez, Bénédicte; Philippot, Pascal; Bonnin-Mosbah, Michelle; Simionovici, Alexandre; Gibert, François

    2002-02-01

    A critical problem for conducting quantitative analysis of individual fluid inclusions using Synchrotron X-Ray Fluorescence (SXRF) technique relates to the standardization and the calibration of the X-ray spectra. In this study, different approaches have been tested for calibration purposes: (a) the use of chlorine when Cl content can be estimated either from melting point depressions of undersaturated fluid inclusions or from saturation limits for halite-bearing fluid inclusions, (b) the use of calcium from synthetic fluid inclusions of known CaCl 2 content as an external standard. SXRF analysis was performed on individual fluid inclusions from the Chivor and Guali emerald deposits, Columbia. These well-known samples contain a single fluid inclusion population for which detailed crush-leach analyses are available, thus providing a relevant compositional reference frame. Concentration estimates were also compared to Particle Induced X-ray Emission (PIXE) analysis carried out independently on the same fluid inclusions. Results of the calibration tests indicate that major (Cl, K, Ca, Fe, Mn) and trace element (Cu, Zn, As, Br, Rb, Sr, Ba, Pb) concentration estimates can be performed without precise knowledge of the analytical volume and the inclusion's 3D geometry. Although the standard deviation of the SXRF results can be relatively high depending on the calibration mode used, mean concentration estimates for most elements are in good agreement with PIXE and crush-leach analysis. Elemental distributions within single fluid inclusions were also established. Associated correlation diagrams argue for the homogeneous distribution of most elements in the fluid inclusion. In contrast, Br shows a bimodal distribution interpreted to reflect a significant enrichment of the vapor portion of the inclusion fluid.

  17. Use of portable X-ray fluorescence instrument for bulk alloy analysis on low corroded indoor bronzes

    Energy Technology Data Exchange (ETDEWEB)

    Šatović, D., E-mail: dsatovic@alu.hr [Department of Conservation and Restoration, Academy of Fine Arts, Ilica 85, 10000 Zagreb (Croatia); Desnica, V. [Department of Conservation and Restoration, Academy of Fine Arts, Ilica 85, 10000 Zagreb (Croatia); Fazinić, S. [Laboratory for Ion Beam Interactions, Ruđer Bošković Institute, Bijenička 54, 10000 Zagreb (Croatia)

    2013-11-01

    One of the most often used non-destructive methods for elemental analysis when performing field measurements on bronze sculptures is X-ray fluorescence (XRF) analysis based on portable instrumentation. However, when performing routine in-situ XRF analysis on corroded objects obtained results are sometimes considerably influenced by the corrosion surface products. In this work the suitability of portable XRF for bulk analysis of low corroded bronzes, which were initially precisely characterized using sophisticated and reliable laboratory methods, was investigated and some improvements in measuring technique and data processing were given. Artificially corroded bronze samples were analyzed by a portable XRF instrument using the same methodology and procedures as when performing in-situ analysis on real objects. The samples were first investigated using sophisticated complementary laboratory techniques: Scanning Electron Microscopy, Proton-Induced X-ray Emission Spectroscopy and Rutherford Backscattering Spectrometry, in order to gain precise information on the formation of the corrosion product layers and in-depth elemental profile of corrosion layers for different aging parameters. It has been shown that for corrosion layers of up to ca. 25 μm a portable XRF can yield very accurate quantification results. - Highlights: • XRF quantification is very accurate for bronze corrosion layers of up to ca. 25 μm. • Corrosion layer formation on bronze described in two phases. • Corrosion layers precisely characterized using PIXE, RBS and SEM. • Corrosion approximated as CuO for layer thickness calculations via X-ray attenuations • Increasingly lighter corrosion matrix may cause SnLα radiation intensity inversion.

  18. Co/Mo2C mirror as studied by x-ray fluorescence and photoelectron spectroscopies induced by x-ray standing waves

    Science.gov (United States)

    Jonnard, P.; Le Guen, K.; Yuan, Y. Y.; André, J.-M.; Mukherjee, S.; Giglia, A.; Nannarone, S.; Mahne, N.; Wang, Z.-S.; Li, H.-C.; Zhu, J.-T.

    2012-12-01

    We study a periodic Co/Mo2C multilayer prepared by magnetron sputtering. The period is 4.1 nm and the sample is designed to work around 778 eV, i.e. close to the Co 2p3/2 threshold, at a glancing angle of 11°. In this condition, strong x-ray standing waves set up within the sample. In order to probe different depths within the stack, particularly the interfaces, the glancing angle is moved along the first Bragg peak, while, the B 1s, C 1s, Mo 3d or O 1s photoelectron spectra, the Co Lα x-ray spectrum as well as the drain current of the sample are measured. Boron is present in the 3.5 nm B4C capping layer and oxygen is from surface contamination. The photoelectrons bring information from the superficial zone, i.e. the 5 first nm, while the characteristic x-rays probe the whole stack. Clear modulations of the intensity of the studied signals as well as core level shifts are observed when going through the Bragg peak. In order to understand what happens in the multilayer calculations of depth distributions of the electric field and the energy loss by the radiation are made with the IMD and OPAL codes, respectively. The combination of experimental results and theoretical simulations will enable us to determine from which place originate the various signals and to know if some interaction exists between the Co and Mo2C layers.

  19. X-ray fluorescence as a method of monitoring metal catalyst content during the purification of carbon nanotubes

    Science.gov (United States)

    Cavness, Brandon; Heimbecker, Joshua; Velasquez, Joe; Williams, S.

    2012-02-01

    There have been several studies that suggest that catalyst metals in carbon nanotubes (CNTs) may pose a health threat. As there are many potential applications of CNTs in medicine, it is important to be able to quantitatively determine the amount of metal catalyst contained in a CNT sample. The relative catalyst content of carbon nanotube samples synthesized via arc-discharge has been determined at various stages of the purification process using X-ray fluorescence (XRF) analysis. Purification was achieved by immersing samples in heated nitric acid. The intensities of the nickel K α X-rays were studied to determine the relative catalyst content in the samples. Scanning electron microscopy (SEM) images of purified nanotubes have been compared to the images of a sample that has been irradiated by 0-15 keV bremsstrahlung in order to determine if the XRF analysis of the nanotubes is in any way destructive. No obvious structural defects were observed as the result of irradiation.

  20. In situ observation of dynamic electrodeposition processes by soft x-ray fluorescence microspectroscopy and keyhole coherent diffractive imaging

    Science.gov (United States)

    Bozzini, Benedetto; Kourousias, George; Gianoncelli, Alessandra

    2017-03-01

    This paper describes two novel in situ microspectroscopic approaches to the dynamic study of electrodeposition processes: x-ray fluorescence (XRF) mapping with submicrometric space resolution and keyhole coherent diffractive imaging (kCDI) with nanometric lateral resolution. As a case study, we consider the pulse-plating of nanocomposites with polypyrrole matrix and Mn x Co y O z dispersoids, a prospective cathode material for zinc-air batteries. This study is centred on the detailed measurement of the elemental distributions developing in two representative subsequent growth steps, based on the combination of in situ identical-location XRF microspectroscopy—accompanied by soft-x ray absorption microscopy—and kCDI. XRF discloses space and time distributions of the two electrodeposited metals and kCDI on the one hand allows nanometric resolution and on the other hand provides complementary absorption as well as phase contrast modes. The joint information derived from these two microspectroscopies allows measurement of otherwise inaccessible observables that are a prerequisite for electrodeposition modelling and control accounting for dynamic localization processes.

  1. Monte Carlo simulation of x-ray fluorescence analysis of gold in kidney using 99mTc radiopharmaceutical

    Science.gov (United States)

    Mahdavi, Naser; Shamsaei, Mojtaba; Shafaei, Mostafa; Rabiei, Ali

    2013-10-01

    The objective of this study was to design a system in order to analyze gold and other heavy elements in internal organs using in vivo x-ray fluorescence (XRF) analysis. Monte Carlo N Particle code MCNP was used to simulate phantoms and sources. A source of 99mTc was simulated in kidney to excite the gold x-rays. Changes in K XRF response due to variations in tissue thickness overlying the kidney at the measurement site were investigated. Different simulations having tissue thicknesses of 20, 30, 40, 50 and 60 mm were performed. Kα1 and Kα2 for all depths were measured. The linearity of the XRF system was also studied by increasing the gold concentration in the kidney phantom from 0 to 500 µg g-1 kidney tissue. The results show that gold concentration between 3 and 10 µg g-1 kidney tissue can be detected for distance between the skin and the kidney surface of 20-60 mm. The study also made a comparison between the skin doses for the source outside and inside the phantom.

  2. Determination of selenium at trace levels in geologic materials by energy-dispersive X-ray fluorescence spectrometry

    Science.gov (United States)

    Wahlberg, J.S.

    1981-01-01

    Low levels of selenium (0.1-500 ppm) in both organic and inorganic geologic materials can be semiquantitatively measured by isolating Se as a thin film for presentation to an energy-dispersive X-ray fluorescence spectrometer. Suitably pulverized samples are first digested by fusing with a mixture of Na2CO3 and Na2O2. The fusion cake is dissolved in distilled water, buffered with NH4Cl, and filtered to remove Si and the R2O3 group. A carrier solution of Na2TeO4, plus solid KI, hydrazine sulfate and Na2SO3, is added to the filtrate. The solution is then vacuum-filtered through a 0.45-??m pore-size filter disc. The filter, with the thin film of precipitate, is supported between two sheets of Mylar?? film for analysis. Good agreement is shown between data reported in this study and literature values reported by epithermal neutron-activation analysis and spectrofluorimetry. The method can be made quantitative by utilizing a secondary precipitation to assure complete recovery of the Se. The X-ray method offers fast turn-around time and a reasonably high production rate. ?? 1981.

  3. Study of on-line analysis using energy dispersive X-ray fluorescence spectrometry for controlling lanthanum and neodymium extraction

    Energy Technology Data Exchange (ETDEWEB)

    Wenli, Li; Ascenzo, G.D`; Curini, R. [Department of Chemistry, University of Rome `La Sapienza`, Rome (Italy); Gasparini, G.M.; Casarci, M.; Mattia, B.; Traverso, D.M.; Bellisario, F. [ENEA, CRE Casaccia INN-NUMA (Italy)

    1998-05-04

    Many rare-earth extraction processes require frequent control over separation process quality. Ideally, an analysis method for this type should be simple, rapid and reliable. Energy dispersive X-ray fluorescence (EDXRF) spectrometry, due to its relative simplicity of instrumentation, speed of analysis, and non-destructive nature, is well suited to this on-line analysis application. In particular, since the radioisotope energy dispersive XRF method eliminates the need to transport samples to a laboratory which houses the X-ray spectrometry, it is most commonly used for on-line analysis of extraction systems. The present paper describes an attempt to type the radioisotope source {sup 241}Am XRF on-line analysis arrangement coupled with a personal computer for controlling a lanthanum and neodymium separation process. From the HpGe detector (high-purity germanium) response, a continuous spectral signal is observed during loading of the feed samples. The separation process using countercurrent extraction consists of a 16-stage laboratory mixer-settler, a switching valve, and a pumping system. The performance of this control system is illustrated by extracting La, Nd acidic solutions with 100% tributyl phosphate

  4. Analytical performance of benchtop total reflection X-ray fluorescence instrumentation for multielemental analysis of wine samples

    Science.gov (United States)

    Dalipi, Rogerta; Marguí, Eva; Borgese, Laura; Bilo, Fabjola; Depero, Laura E.

    2016-06-01

    Recent technological improvements have led to a widespread adoption of benchtop total reflection X-ray fluorescence systems (TXRF) for analysis of liquid samples. However, benchtop TXRF systems usually present limited sensitivity compared with high-scale instrumentation which can restrict its application in some fields. The aim of the present work was to evaluate and compare the analytical capabilities of two TXRF systems, equipped with low power Mo and W target X-ray tubes, for multielemental analysis of wine samples. Using the Mo-TXRF system, the detection limits for most elements were one order of magnitude lower than those attained using the W-TXRF system. For the detection of high Z elements like Cd and Ag, however, W-TXRF remains a very good option due to the possibility of K-Lines detection. Accuracy and precision of the obtained results have been evaluated analyzing spiked real wine samples and comparing the TXRF results with those obtained by inductively coupled plasma emission spectroscopy (ICP-OES). In general, good agreement was obtained between ICP-OES and TXRF results for the analysis of both red and white wine samples except for light elements (i.e., K) which TXRF concentrations were underestimated. However, a further achievement of analytical quality of TXRF results can be achieved if wine analysis is performed after dilution of the sample with de-ionized water.

  5. CHARACTERIZATION OF SALT PARTICLE INDUCED CORROSION PROCESSES BY SYNCHROTRON GENERATED X-RAY FLUORESCENCE AND COMPLEMENTARY SURFACE ANALYSIS TOOLS.

    Energy Technology Data Exchange (ETDEWEB)

    NEUFELD, A.K.; COLE, I.S.; BOND, A.M.; ISAACS, H.S.; FURMAN, S.A.

    2001-03-25

    The benefits of using synchrotron-generated X-rays and X-ray fluorescence analysis in combination with other surface analysis techniques have been demonstrated. In studies of salt-induced corrosion, for example, the detection of Rb ions in the area of secondary spreading when salt-containing micro-droplets are placed on zinc surfaces, further supports a mechanism involving cation transport during the corrosion and spreading of corrosive salt on exposed metal surfaces. Specifically, the new analytical data shows that: (a) cations are transported radially from a primary drop formed from a salt deposit in a thin film of secondary spreading around the drop; (b) subsequently, micro-pools are formed in the area of secondary spreading, and it is likely that cations transported within the thin film accumulate in these micro-pools until the area is dehydrated; (c) the mechanism of cation transport into the area of secondary spreading does not include transport of the anions; and (d) hydroxide is the counter ion formed from oxygen reduction at the metal surface within the spreading layer. Data relevant to iron corrosion is also presented and the distinct differences relative to the zinc situation are discussed.

  6. On the Detectability of Oxygen X-ray Fluorescence and its Use as a Solar Photospheric Abundance Diagnostic

    CERN Document Server

    Drake, Jeremy J

    2008-01-01

    Monte Carlo calculations of the O Kalpha line fluoresced by coronal X-rays and emitted just above the temperature minimum region of the solar atmosphere have been employed to investigate the use of this feature as an abundance diagnostic. While quite weak, we estimate line equivalent widths in the range 0.02-0.2 AA, depending on the X-ray plasma temperature. The line remains essentially uncontaminated by blends for coronal temperatures T =~ 2 ph/s/arcmin^2. Model calculations for solar chemical mixtures with an O abundance adjusted up and down by a factor of 2 indicate 35-60% changes in O Kalpha line equivalent width, providing a potentially useful O abundance diagnostic. Sensitivity of equivalent width to differences between recently recommended chemical compositions with ``high'' and ``low'' complements of the CNO trio important for interpreting helioseismological observations is less accute, amounting to 20-26% at coronal temperatures T ~= 1000 and suitably well-behaved instrumental profile can be built, X...

  7. Grazing incidence X-ray fluorescence analysis of buried interfaces in periodically structured crystalline silicon thin-film solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Eisenhauer, David; Preidel, Veit; Becker, Christiane [Young Investigator Group Nanostructured Silicon for Photovoltaic and Photonic Implementations (Nano-SIPPE), Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Berlin (Germany); Pollakowski, Beatrix; Beckhoff, Burkhard [Physikalisch-Technische Bundesanstalt, Berlin (Germany); Baumann, Jonas; Kanngiesser, Birgit [Institut fuer Optik und Atomare Physik, Technische Universitaet Berlin (Germany); Amkreutz, Daniel; Rech, Bernd [Institut Silizium Photovoltaik, Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Berlin (Germany); Back, Franziska; Rudigier-Voigt, Eveline [SCHOTT AG, Mainz (Germany)

    2015-03-01

    We present grazing incidence X-ray fluorescence (GIXRF) experiments on 3D periodically textured interfaces of liquid phase crystallized silicon thin-film solar cells on glass. The influence of functional layers (SiO{sub x} or SiO{sub x}/SiC{sub x}) - placed between glass substrate and silicon during crystallization - on the final carbon and oxygen contaminations inside the silicon was analyzed. Baring of the buried structured silicon surface prior to GIXRF measurement was achieved by removal of the original nano-imprinted glass substrate by wet-chemical etching. A broad angle of incidence distribution was determined for the X-ray radiation impinging on this textured surface. Optical simulations were performed in order to estimate the incident radiation intensity on the structured surface profile considering total reflection and attenuation effects. The results indicate a much lower contamination level for SiO{sub x} compared to the SiO{sub x}/SiC{sub x} interlayers, and about 25% increased contamination when comparing structured with planar silicon layers, both correlating with the corresponding solar cell performances. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. X-ray fluorescence analysis of Mexican varieties of dried chili peppers II: Commercial and home-grown specimens

    Science.gov (United States)

    Romero-Dávila, E.; Miranda, J.; Pineda, J. C.

    2015-07-01

    Elemental analyses of samples of Mexican varieties of dried chili peppers were carried out using X-ray Fluorescence (XRF). Several specimens of Capsicum annuum L., Capsicum chinense, and Capsicum pubescens were analyzed and the results compared to previous studies of elemental contents in other varieties of Capsicum annuum (ancho, morita, chilpotle, guajillo, pasilla, and árbol). The first set of samples was bought packaged in markets. In the present work, the study focuses on home-grown samples of the árbol and chilpotle varieties, commercial habanero (Capsicum chinense), as well as commercial and home-grown specimens of manzano (Capsicum pubescencs). Samples were freeze dried and pelletized. XRF analyses were carried out using a spectrometer based on an Rh X-ray tube, using a Si-PIN detector. The system detection calibration was performed through the analysis of the NIST certified reference materials 1547 (peach leaves) and 1574 (tomato leaves), while accuracy was checked with the reference material 1571 (orchard leaves). Elemental contents of all elements in the new set of samples were similar to those of the first group. Nevertheless, it was found that commercial samples contain high amounts of Br, while home-grown varieties do not.

  9. SMM observations of K-alpha radiation from fluorescence of photospheric iron by solar flare X-rays

    Science.gov (United States)

    Parmar, A. N.; Culhane, J. L.; Rapley, C. G.; Wolfson, C. J.; Acton, L. W.; Phillips, K. J. H.; Dennis, B. R.

    1984-01-01

    High-resolution Fe K-alpha spectra near 1.94 A observed during solar flares with the Bent Crystal Spectrometer on the Solar Maximum Mission are presented. The evidence for two possible excitation mechanisms, electron impact and fluorescence, is examined. It is found that the fluorescence mechanism satisfactorily describes the results, while the observations do not support electron collisional excitation of the Fe K-alpha transitions in low ionization stages (II-XII) of iron. Using Bai's model of the fluorescent excitation process, the photospheric iron abundance relative to that of hydrogen is estimated to be 5-6 x 10 to the -5th. The mean height of the soft X-ray source producing the K-alpha fluorescence is calculated on the basis of this model for about 40 large flares. The solar K-alpha lines are found to be about 25 percent wider than those measured in the laboratory. Weak line features observed at wavelengths shorter than that of the K-alpha lines are discussed.

  10. Gold nephropathy. Ultrastructural, fluorescent, and energy-dispersive x-ray microanalysis study

    Energy Technology Data Exchange (ETDEWEB)

    Ainsworth, S.K.; Swain, R.P.; Watabe, N.; Brackett, N.C. Jr.; Pilia, P.; Hennigar, G.R.

    1981-07-01

    The nephrotic syndrome developed in a patient receiving therapy with gold for rheumatoid arthritis. The results of a histopathological examination of the renal biopsy specimen were unremarkable. Immunofluorescent studies showed deposits of immunoglobulins and C3 in a granular pattern in the glomerular basement membranes. Ultrastructurally, the discrete osmiophilic immune complexes were epimembranous. By x-ray microanalysis, gold that was complexed with sulfur was present in proximal tubular cytoplasmic vacuoles and nuclei. Gold and sulfur could not be demonstrated in glomerular epimembranous deposits. The results of these studies suggest that immune complex deposition does not involve gold and sulfur acting as haptens. Gold-salt therapy may result in damage to proximal tubules that leak renal tubular antigens, which in turn complex with autoantibody and produce an autoimmune membranous nephropathy. The evidence for this mechanism is not convincing. Although the data indicate an immune-complex cause for gold-salt nephropathy, the incident antigen (or antigens) and mechanism of action remain unidentified.

  11. Energy-dispersive X-ray fluorescence – A tool for interdisciplinary research

    Indian Academy of Sciences (India)

    M Sudarshan; S S Ram; S Majumdar; J P Maity; J G Ray; A Chakraborty

    2011-02-01

    Trace elements have been at the focus of attention for decades with considerable emphasis on their role in biology and biomedical sciences, environmental sciences, geology, archaeology and material sciences. They comprise a large number of elements, some having essential physiological functions, whereas others are toxic, mutagenic or carcinogenic. A few even have antiproliferative and anticarciniogenic properties. The advent of various instrumental techniques and sophisticated instrumentations has made their detection to very low limits possible, making this a very important multidisciplinary study. Among these techniques the energy-dispersive X-ray fluorescence (EDXRF) technique is being widely used for trace element detection in various fields of science. Keeping the importance of trace elements in mind, the Kolkata centre of UGC-DAE Consortium for Scientific Research initiated several research schemes in different fields of trace element research using various techniques, EDXRF being one of the main techniques. A Xenemetrix (erstwhile Jordan Valley) EX 3600 EDXRF spectrometer is being used to carry out the research. This presentation aims to highlight some of the very recent applications of EDXRF in the study of the role of trace elements in pre-cancerous tissues, medicinal plants and also in some environmental studies.

  12. Nanodroplet quantification: pushing the detection limits of micro x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Miller, T. C. (Thomasin C.); Havrilla, G. J. (George J.)

    2002-01-01

    In this study, detection limits for a variety of elements were determined on an EDAX Eagle I1 MXRF system equipped with a polycapillary and a Rh X-ray source. Both mass, volume, and spot diameter detection limits were established using dried spot technology, where various volumes and/or masses of different elements were deposited on different substrates, dried, and quantitatively analyzed by MXRF. Preliminary results have shown that sub-nanogram levels of material can be detected in less than 200 pm diameter spot sizes deposited on thin polymer films. Specifically, detection limits were found for a given element as a function of mass deposited for a given spot volume, and volume deposited for a given mass. The effect of the presence of multiple elements in a droplet on the detection limit was also investigated. For example, the detection limit for copper was determined when it was deposited as a single Cu solution and in various multielement mixtures containing from 2 up to 10 different elements. To determine how the substrate affects the detection limit of different species, elemental dried spots were analyzed on different polymer films, including polypropylene and AP 1 . Comparisons were also made to elements deposited on different spherical, resin substrates such as polystyrene beads.

  13. Using Nondestructive Portable X-ray Fluorescence Spectrometers on Stone, Ceramics, Metals, and Other Materials in Museums: Advantages and Limitations.

    Science.gov (United States)

    Tykot, Robert H

    2016-01-01

    Elemental analysis is a fundamental method of analysis on archaeological materials to address their overall composition or identify the source of their geological components, yet having access to instrumentation, its often destructive nature, and the time and cost of analyses have limited the number and/or size of archaeological artifacts tested. The development of portable X-ray fluorescence (pXRF) instruments over the past decade, however, has allowed nondestructive analyses to be conducted in museums around the world, on virtually any size artifact, producing data for up to several hundred samples per day. Major issues have been raised, however, about the sensitivity, precision, and accuracy of these devices, and the limitation of performing surface analysis on potentially heterogeneous objects. The advantages and limitations of pXRF are discussed here regarding archaeological studies of obsidian, ceramics, metals, bone, and painted materials.

  14. Provenance studies of archaeological ceramics from Mar-Takla (Ain-Minin, Syria) using radioisotope X-ray fluorescence method

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The radioisotope X-ray fluorescence method was applied to studies of the provenance of the ceramics fragments originated from the Mar-Takla site in Syria. The samples were irradiated 1000s by a 109Cd radioisotope source and 13 elements (Ca, Ti, Mn, Fe, Zn, Ga, As, Rb, Sr, Y, Zr, Nb, and Pb) were determined in 35 samples. The data were subjected to two multivariate statistical methods, cluster and principal components analysis (PCA). It was shown from the combination of the statistical techniques and the determination of elemental composition of the samples that 94% of the ceramic samples analyzed can be considered to be manufactured using two sources of raw materials.

  15. Rapid detection of toxic metals in non-crushed oyster shells by portable X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Chou Ju, E-mail: Ju.Chou@selu.ed [Department of Chemistry and Physics, Southeastern Louisiana University, Hammond, LA 70402 (United States); Clement, Garret; Bursavich, Bradley; Elbers, Don [Department of Chemistry and Physics, Southeastern Louisiana University, Hammond, LA 70402 (United States); Cao Baobao; Zhou Weilie [Advanced Material Research Institute, University of New Orleans, New Orleans, LA 70148 (United States)

    2010-06-15

    The aim of this study was the multi-elemental detection of toxic metals such as lead (Pb) in non-crushed oyster shells by using a portable X-ray fluorescence (XRF) spectrometer. A rapid, simultaneous multi-element analytical methodology for non-crushed oyster shells has been developed using a portable XRF which provides a quick, quantitative, non-destructive, and cost-effective mean for assessment of oyster shell contamination from Pb. Pb contamination in oyster shells was further confirmed by scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). The results indicated that Pb is distributed in-homogeneously in contaminated shells. Oyster shells have a lamellar structure that could contribute to the high accumulation of Pb on oyster shells. - A rapid, simultaneous multi-element analytical methodology for non-crushed oyster shells has been developed using XRF and contamination of lead on oyster shells was confirmed by XRF and SEM-EDS.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  17. Individual particle analysis of coarse air suspended particulate material by synchrotron radiation X-ray micro fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Melo Junior, Ariston [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Perez, Carlos Alberto [Laboratorio Nacional de Luz Sincrotron (LNLS), Campinas, SP (Brazil)]. E-mail: perez@lnls.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br

    2005-07-01

    The purpose of this work is evaluate the size of individual particles present in the air suspended particulate material collected in Campinas, Sao Paulo State, and analyze quantitatively the particles using the synchrotron radiation X-ray micro fluorescence ({mu}-SRXRF) associated with the fundamental parameter method to correct attenuation/absorption effects by the matrix. The particles analyzed have size between 50-10 {mu}m and to perform the spatial distribution a white beam of synchrotron radiation condensed by a conical capillary (13 {mu}m diameter) was used. For the quantitative analysis punctual measures in thin films standards in Mylar subtract were performed. The elements detected were Si, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb. (author)

  18. Dendrochemical patterns of calcium, zinc, and potassium related to internal factors detected by energy dispersive X-ray fluorescence (EDXRF)

    Science.gov (United States)

    Smith, Kevin T.; Balouet, Jean Christophe; Shortle, Walter C.; Chalot, Michel; Beaujard, François; Grudd, Håkan; Vroblesky, Don A.; Burkem, Joel G.

    2014-01-01

    Energy dispersive X-ray fluorescence (EDXRF) provides highly sensitive and precise spatial resolution of cation content in individual annual growth rings in trees. The sensitivity and precision have prompted successful applications to forensic dendrochemistry and the timing of environmental releases of contaminants. These applications have highlighted the need to distinguish dendrochemical effects of internal processes from environmental contamination. Calcium, potassium, and zinc are three marker cations that illustrate the influence of these processes. We found changes in cation chemistry in tree rings potentially due to biomineralization, development of cracks or checks, heartwood/sapwood differentiation, intra-annual processes, and compartmentalization of infection. Distinguishing internal from external processes that affect dendrochemistry will enhance the value of EDXRF for both physiological and forensic investigations.

  19. Trace element analyses of spheres from the melt zone of the Greenland ice cap using synchrotron X ray fluorescence

    Science.gov (United States)

    Chevallier, P.; Wang, J.; Jehanno, C.; Maurette, M.; Sutton, S. R.

    1986-01-01

    Synchrotron X-ray fluorescence spectra of unpolished iron and chondritic spheres extracted from sediments collected on the melt zone of the Greenland ice cap allow the analysis of Ni, Cu, Zn, Ga, Ge, Pb, and Se with minimum detection limits on the order of several parts per million. All detected elements are depleted relative to chondritic abundance with the exception of Pb, which shows enrichments up to a factor of 500. An apparent anticorrelation between the Ni-content and trace element concentration was observed in both types of spherules. The fractionation patterns of the iron and chondritic spheres are not complementary and consequently the two iron spheres examined in this study are unlikely to result from ejection of globules of Fe/Ni from parent chondritic micrometeoroids.

  20. Development of a Silicon Drift Detector Array: An X-ray Fluorescence Spectrometer for Remote Surface Mapping

    Energy Technology Data Exchange (ETDEWEB)

    Gaskin, J.A.; De Geronimo, G.; Carini, G.A.; Chen, W.; Elsner, R.F.; Kramer, G.; Keister, J.W.; Li, Z.; Ramsey, B.D.; Rehak, P.; Siddons, D.P.

    2009-09-11

    Over the past three years NASA Marshall Space Flight Center has been collaborating with Brookhaven National Laboratory to develop a modular Silicon Drift Detector (SDD) X-Ray Spectrometer (XRS) intended for fine surface mapping of the light elements of the moon. The value of fluorescence spectrometry for surface element mapping is underlined by the fact that the technique has recently been employed by three lunar orbiter missions; Kaguya, Chandrayaan-1, and Chang'e. The SDD-XRS instrument we have been developing can operate at a low energy threshold (i.e. is capable of detecting Carbon), comparable energy resolution to Kaguya (<150 eV at 5.9 keV) and an order of magnitude lower power requirement, making much higher sensitivities possible. Furthermore, the intrinsic radiation resistance of the SDD makes it useful even in radiation-harsh environments such as that of Jupiter and its surrounding moons.

  1. X-ray fluorescence-based method for the quantitative determination of uranium in the aqueous solutions

    Science.gov (United States)

    Dubrovka, S.; Chursin, S.; Verkhoturova, V.

    2017-01-01

    Currently, one of the important issues in the field of nuclear technology is providing special handling with respect to nuclear materials, due to their energy and commercial significancy, as well as their potential radiation contamination threat. There is a necessity to have information about the full qualitative and quantitative composition of the sample as a part of special handling with nuclear materials. Spectrometric methods solve this problem effectively. One of these methods is the X-ray fluorescence analysis, which is fast, nondestructive and environmentally friendly with a high accuracy and reproducibility of the results. Development of uranium quantitative determination method in aqueous solutions to solve the problems of accounting and control of nuclear materials is the subject of research in this article. The development of the uranium concentration determination method in the aqueous solutions of uranyl nitrate UO2(NO3)2 was carried out using Spectroscan MAKC-G – wavelength dispersive crystal diffraction XRF spectrometer.

  2. Non-destructive analysis of didymium and praseodymium molybdate crystals using energy dispersive X-ray fluorescence technique

    Science.gov (United States)

    Bhat, C. K.; Joseph, Daisy; Pandita, Sanjay; Kotru, P. N.

    2016-08-01

    Analysis of didymium (Di) and praseodymium molybdate crystals were carried out using energy dispersive X-ray fluorescence (EDXRF). The assigned empirical chemical formulae of the composites were tested and verified by the EDXRF technique by estimating experimental major elemental concentration ratios. On the Basis of these ratios, the established formulae for some of the composite materials have been verified and suggestions made for their refinement. Non-destructive technique used in this analysis enables to retain the original crystal samples and makes rapid simultaneous scan of major elements such as La, Pr, Ned and Mo as well as impurities such as Ce. Absence of samarium(Sm) in the spectrum during analysis of didymium molybdate crystals indicated an incomplete growth of mixed rare earth single crystal. These crystals (e.g.,Di) are shown to be of modified stoichiometry with Ce as trace impurity.

  3. Analysis of pre-Islamic ceramics from the Kur River Basin (Fars, Iran) using handheld X-ray fluorescence spectrometry

    Science.gov (United States)

    Pincé, Possum; Vekemans, Bart; Vandenabeele, Peter; Haerinck, Ernie; Overlaet, Bruno

    2016-09-01

    A large number of painted pre-Islamic ceramics from the Kur River Basin (Fars province, Iran) was collected on surveys and excavations conducted by the late Prof. L. Vanden Berghe (Ghent University, Belgium) during the 1950s. Handheld X-ray fluorescence spectrometry was undertaken on a selection of these ceramics to evaluate the applicability of the technique to study the fabric of these ceramics and the pigments used for decoration. The aim is to obtain elemental data, from which information about raw materials, manufacturing techniques and exchange systems can be extracted. A total of 26 sherds was analyzed dating from the Neolithic to the Late Bronze Age and belonging to different sites and styles. Five compositional groups could be identified in the dataset. These elemental groups differ from the groups obtained by the macroscopic study and are related to the production process and/or the provenance of the primary materials.

  4. Raman microscopy and x-ray fluorescence analysis of pigments on medieval and Renaissance Italian manuscript cuttings.

    Science.gov (United States)

    Burgio, Lucia; Clark, Robin J H; Hark, Richard R

    2010-03-30

    Italian medieval and Renaissance manuscript cuttings and miniatures from the Victoria and Albert Museum were analyzed by Raman microscopy to compile a database of pigments used in different periods and different Italian regions. The palette identified in most manuscripts and cuttings was found to include lead white, gypsum, azurite, lazurite, indigo, malachite, vermilion, red lead, lead tin yellow (I), goethite, carbon, and iron gall ink. A few of the miniatures, such as the historiated capital "M" painted by Gerolamo da Cremona and the Petrarca manuscript by Bartolomeo Sanvito, are of exceptional quality and were analyzed extensively; some contained unusual materials. The widespread usage of iron oxides such as goethite and hematite as minor components of mixtures with azurite is particularly notable. The use of a needle-shaped form of iron gall ink as a pigment rather than a writing material was established by both Raman microscopy and x-ray fluorescence spectroscopy for the Madonna and Child by Franco de' Russi.

  5. Implementation of X-ray fluorescence microscopy for investigation of elemental abnormalities in central nervous system tissue

    Energy Technology Data Exchange (ETDEWEB)

    Chwiej, J. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland)]. E-mail: jchwiej@novell.ftj.agh.edu.pl; Szczerbowska-Boruchowska, M. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Wojcik, S. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Lankosz, M. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Chlebda, M. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Adamek, D. [Institute of Neurology, Collegium Medicum, Jagiellonian University, ul. Botaniczna-3, 31-503 Cracow (Poland); Tomik, B. [Institute of Neurology, Collegium Medicum, Jagiellonian University, ul. Botaniczna-3, 31-503 Cracow (Poland); Setkowicz, Z. [Department of Neuroanatomy, Institute of Zoology, Jagiellonian University, ul. Ingardena 6, 30-060 Cracow (Poland); Falkenberg, G. [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, Hamburg (Germany); Stegowski, Z. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Szczudlik, A. [Institute of Neurology, Collegium Medicum, Jagiellonian University, ul. Botaniczna-3, 31-503 Cracow (Poland)

    2005-09-29

    The microbeam synchrotron radiation X-ray fluorescence technique (micro-SRXRF) was applied to topographic and quantitative elemental analysis of human spinal cord tissue sections. The feasibility of this technique for the determination of elemental abnormalities caused by neurodegenerative disorder, i.e. amyotrophic lateral sclerosis (ALS), was verified. The applied measurement conditions allowed detecting: P, S, Cl, K, Ca, Fe, Cu, Zn and Br in thin tissue slices. Two-dimensional maps of the elemental distribution were recorded. Quantitative differences in elemental concentration between gray matter, nerve cells and white matter were observed for all analyzed cases. For the motor neuron bodies higher accumulation of S, Cl, K, Fe, Zn and Br was noticed. The results showed significant differences of elemental accumulation between the analyzed ALS cases. Moreover, the feasibility of using tissue sections fixed and embedded in paraffin for micro-SRXRF analysis was tested. These studies were performed on the samples of rat brain.

  6. Practical guidelines for best practice on Total Reflection X-ray Fluorescence spectroscopy: Analysis of aqueous solutions

    Science.gov (United States)

    Riaño, Sofía; Regadío, Mercedes; Binnemans, Koen; Vander Hoogerstraete, Tom

    2016-10-01

    Despite the fact that Total Reflection X-ray Fluorescence (TXRF) is becoming more and more popular as a quantification technique in analytical chemistry due to its simplicity and robustness, there are still some key aspects related to the sample preparation that need to be improved. In this work, the effect of different parameters is investigated: measurement time, carrier position, sample volume and sample drying time. The measurement time and the sample volume on the carriers mainly affect the recovery rate and relative standard deviation of the quantified metal from aqueous solutions. The most important parameters that play a fundamental role in the calibration of a TXRF machine such as choice of the standard element and concentration ratio between the analyte and the standard are discussed. Practical and easy guidelines for the correct preparation of aqueous samples are presented. These can be used by both less and more experienced TXRF users, interested in measuring metal ion concentrations in aqueous samples.

  7. Rapid determination of silver in nanobased liquid dietary supplements using a portable X-ray fluorescence analyzer.

    Science.gov (United States)

    Sánchez-Pomales, Germarie; Mudalige, Thilak K; Lim, Jin-Hee; Linder, Sean W

    2013-07-31

    This paper reports a rapid and straightforward method for the quantitation of total Ag content in nanobased commercially available liquid dietary supplements using a portable X-ray fluorescence (pXRF) analyzer. Figures of merits were evaluated by analyzing a series of AgNO3 standards. This method was shown to have a detection limit of 3 ppm, a quantitation limit of 10 ppm, and a broad linear range from the detection limit to 10000 ppm (1%). Accurate detection and quantitation of Ag content in well-characterized Ag nanoparticle samples and in nanobased liquid dietary supplements were achieved with good correlation (i.e., percentage difference average values under 15%) between the total Ag concentration obtained by the pXRF analyzer and by inductively coupled plasma mass spectrometry (ICP-MS). Furthermore, accurate quantitation of Ag in the presence of high concentrations of potential spectral interferences was also demonstrated.

  8. X-ray fluorescence and imaging analyses of paintings by the Brazilian artist Oscar Pereira Da Silva

    Science.gov (United States)

    Campos, P. H. O. V.; Kajiya, E. A. M.; Rizzutto, M. A.; Neiva, A. C.; Pinto, H. P. F.; Almeida, P. A. D.

    2014-02-01

    Non-destructive analyses, such as EDXRF (Energy-Dispersive X-Ray Fluorescence) spectroscopy, and imaging were used to characterize easel paintings. The analyzed objects are from the collection of the Pinacoteca do Estado de São Paulo. EDXRF results allowed us to identify the chemical elements present in the pigments, showing the use of many Fe-based pigments, modern pigments, such as cobalt blue and cadmium yellow, as well as white pigments containing lead and zinc used by the artist in different layers. Imaging analysis was useful to identify the state of conservation, the localization of old and new restorations and also to detect and unveil the underlying drawings revealing the artist's creative processes.

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

    Science.gov (United States)

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

    2016-10-01

    In this study, total reflection x-ray fluorescent (TXRF) spectrometry was applied for the evaluation of iron concentration in ferrofluids and biological samples containing iron oxide magnetic nanoparticles obtained by the laser target evaporation technique. Suspensions of maghemite nanoparticles of different concentrations were used to estimate the limitation of the method for the evaluation of nanoparticle concentration in the range of 1-5000 ppm in absence of organic matrix. Samples of single-cell yeasts grown in the nutrient media containing maghemite nanoparticles were used to study the nanoparticle absorption mechanism. The obtained results were analyzed in terms of applicability of TXRF for quantitative analysis in a wide range of iron oxide nanoparticle concentrations for biological samples and ferrofluids with a simple established protocol of specimen preparation.

  10. Carbon nanotubes allow capture of krypton, barium and lead for multichannel biological X-ray fluorescence imaging

    Science.gov (United States)

    Serpell, Christopher J.; Rutte, Reida N.; Geraki, Kalotina; Pach, Elzbieta; Martincic, Markus; Kierkowicz, Magdalena; de Munari, Sonia; Wals, Kim; Raj, Ritu; Ballesteros, Belén; Tobias, Gerard; Anthony, Daniel C.; Davis, Benjamin G.

    2016-10-01

    The desire to study biology in situ has been aided by many imaging techniques. Among these, X-ray fluorescence (XRF) mapping permits observation of elemental distributions in a multichannel manner. However, XRF imaging is underused, in part, because of the difficulty in interpreting maps without an underlying cellular `blueprint' this could be supplied using contrast agents. Carbon nanotubes (CNTs) can be filled with a wide range of inorganic materials, and thus can be used as `contrast agents' if biologically absent elements are encapsulated. Here we show that sealed single-walled CNTs filled with lead, barium and even krypton can be produced, and externally decorated with peptides to provide affinity for sub-cellular targets. The agents are able to highlight specific organelles in multiplexed XRF mapping, and are, in principle, a general and versatile tool for this, and other modes of biological imaging.

  11. Development of a Silicon Drift Detector Array: An X-Ray Fluorescence Spectrometer for Remote Surface Mapping

    Science.gov (United States)

    Gaskin, Jessica A.; Carini, Gabriella A.; Wei, Chen; Elsner, Ronald F.; Kramer, Georgiana; De Geronimo, Gianluigi; Keister, Jeffrey W.; Zheng, Li; Ramsey, Brian D.; Rehak, Pavel; Siddons, D. Peter

    2009-01-01

    Over the past three years NASA Marshall Space Flight Center has been collaborating with Brookhaven National Laboratory to develop a modular Silicon Drift Detector (SDD) X-Ray Spectrometer (XRS) intended for fine surface mapping of the light elements of the moon. The value of fluorescence spectrometry for surface element mapping is underlined by the fact that the technique has recently been employed by three lunar orbiter missions; Kaguya, Chandrayaan-1, and Chang e. The SDD-XRS instrument we have been developing can operate at a low energy threshold (i.e. is capable of detecting Carbon), comparable energy resolution to Kaguya (SDD makes it useful even in radiation-harsh environments such as that of Jupiter and its surrounding moons.

  12. Design and optimization of an analog filter with a CdTe detector for X-ray fluorescence applications

    Science.gov (United States)

    Choi, Hyojeong; Kim, Hui Su; Kim, Young Soo; Ha, Jang Ho; Chai, Jong-Seo

    2016-10-01

    An analog pre-filter circuit for digital pulse processing is designed and optimized for X-ray fluorescence (XRF) applications to replace traditional analog shaping amplifiers. To optimize the pre-filter performance, we characterized noise electrons as a function of the input pulse rise time and decay time of the output pulse by using the full width at half maximum. In addition, gamma-ray energy measurements at room temperature showed that the commercially available CdTe Schottky-type radiation detector with our newly designed and optimized pre-filter circuit exhibited full widths at half maxima of 4.97 (Ba-133, at 53 keV) and 5.56 keV (Am-241, at 59.5 keV), respectively.

  13. Defect detection inside superconducting 1.3 GHz cavities by means of x-ray fluorescence spectroscopy

    Science.gov (United States)

    Bertucci, M.; Michelato, P.; Moretti, M.; Navitski, A.; Pagani, C.

    2016-01-01

    X-ray fluorescence probe for detection of foreign material inclusions on the inner surface of superconducting cavities has been developed and tested. The setup detects trace element content such as a few micrograms of impurities responsible for thermal breakdown phenomena limiting the cavity performance. The setup has been customized for the geometry of 1.3 GHz TESLA-type niobium cavities and focuses on the surface of equator area at around 103 mm from the centre axis of the cavities with around 20 mm detection spot. More precise localization of inclusions can be reconstructed by means of angular or lateral displacement of the cavity. Preliminary tests confirmed a very low detection limit for elements laying in the high efficiency spectrum zone (from 5 to 10 keV), and a high angular resolution allowing an accurate localization of defects within the equator surface.

  14. Application of X-Ray Fluorescence Analysis to Determine the Elemental Composition of Tissues from Different Ovarian Neoplasms

    Science.gov (United States)

    Motevich, I. G.; Strekal, N. D.; Papko, N. M.; Glebovich, M. I.; Shulha, A. V.; Maskevich, S. A.

    2015-03-01

    We present the results of x-ray fluorescence analysis of tissues from healthy ovaries and from ovaries with different pathologies: benign and borderline tumors, mucinous and endometrioid cancers, serous carcinomas. We determine the average copper, zinc, calcium, selenium, cadmium, lead, and mercury levels. We observed that in the benign ovarian tumors, we see a significant decrease in the cadmium, mercury, and lead levels compared with healthy tissues. In the borderline neoplasms, the copper level is reduced relative to zinc (Cu/Zn), cadmium, mercury, and lead, and also the zinc concentration is increased. In the ovarian carcinomas, we observed changes in the ratio of the chemical elements in the tumor tissues, depending on the histologic type. The results obtained can be used for differentiation, diagnosis, and adjustment of treatment for different ovarian neoplasms.

  15. Green copper pigments biodegradation in cultural heritage: from malachite to moolooite, thermodynamic modeling, X-ray fluorescence, and Raman evidence.

    Science.gov (United States)

    Castro, Kepa; Sarmiento, Alfredo; Martínez-Arkarazo, Irantzu; Madariaga, Juan Manuel; Fernández, Luis Angel

    2008-06-01

    Moolooite (copper oxalate), a very rare compound, was found as a degradation product from the decay of malachite in several specimens of Cultural Heritage studied. Computer simulations, based on heterogeneous chemical equilibria, support the transformation of malachite to moolooite through the intermediate copper basic sulfates or copper basic chlorides, depending on the presence of available free sulfate or chloride anions in the chemical system. Raman and X-ray fluorescence spectral evidence found during the analysis of the three case studies investigated supported the model predictions. According to the study, the presence of lichens and other microorganisms might be responsible for the decay phenomena. This work tries to highlight the importance of biological attack on specimens belonging to Cultural Heritage and to demonstrate the consequences of oxalic acid, excreted by some of these microorganisms, on the conservation and preservation of artwork.

  16. Rapid detection of toxic metals in non-crushed oyster shells by portable X-ray fluorescence spectrometry.

    Science.gov (United States)

    Chou, Ju; Clement, Garret; Bursavich, Bradley; Elbers, Don; Cao, Baobao; Zhou, Weilie

    2010-06-01

    The aim of this study was the multi-elemental detection of toxic metals such as lead (Pb) in non-crushed oyster shells by using a portable X-ray fluorescence (XRF) spectrometer. A rapid, simultaneous multi-element analytical methodology for non-crushed oyster shells has been developed using a portable XRF which provides a quick, quantitative, non-destructive, and cost-effective mean for assessment of oyster shell contamination from Pb. Pb contamination in oyster shells was further confirmed by scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). The results indicated that Pb is distributed in-homogeneously in contaminated shells. Oyster shells have a lamellar structure that could contribute to the high accumulation of Pb on oyster shells.

  17. Integrating X-ray fluorescence and infrared imaging microspectroscopies for comprehensive characterization of an acetaminophen model pharmaceutical.

    Science.gov (United States)

    Patterson, Brian M; Havrilla, George J

    2006-05-01

    The integration of full spectral images using the complementary microspectroscopic imaging techniques X-ray fluorescence and Fourier transform infrared is demonstrated. This effort surpasses previous work in that a single chemometric software package is used to elicit chemical information from the integrated spectroscopic images. Integrating these two complementary spectroscopic methods provides both elemental and molecular spatial distribution within a specimen. The critical aspect in this work is using full spectral maps from each pixel within the image and subsequent processing with chemometric tools to provide integrated chemical information. This integration enables a powerful approach to more comprehensive materials characterization. Issues addressed include sample registration and beam penetration depth and how each affects post-processing. An inorganic salt and an acetaminophen pharmaceutical model mixture demonstrate the power of integrating these techniques with chemometric software.

  18. Micro-X-ray fluorescence as a general high-throughput screening method for catalyst discovery and small molecule recognition.

    Science.gov (United States)

    Miller, Thomasin C; Mann, Grace; Havrilla, George J; Wells, Cyndi A; Warner, Benjamin P; Baker, R Tom

    2003-01-01

    A powerful high-throughput screening technique is described for the rapid screening of bead-based libraries for catalyst discovery and molecular recognition. Micro-X-ray fluorescence (MXRF) screens materials for elemental composition with mesoscale analysis. This method is nondestructive and requires minimal sample preparation and no special tags for analysis, and the screening time is dependent on the desired sensitivity. The speed, sensitivity, and simplicity of MXRF as a high-throughput screening technique were applied to screen bead-based libraries of oligopeptides for phosphate hydrolysis catalysts and molecular recognition of selective receptors for the degradation products and analogues of chemical warfare agents. This paper demonstrates the analytical or HTS capability of MXRF for combinatorial screening. It is meant only to show the capabilities of MXRF and is not meant as an exhaustive study of the catalyst and molecular recognition systems presented.

  19. Waste reduction process improvements in the analysis of plutonium by x-ray fluorescence: results from multiple data sets

    Energy Technology Data Exchange (ETDEWEB)

    Worley, Christopher G [Los Alamos National Laboratory; Soderberg, Constance B [Los Alamos National Laboratory; Townsend, Lisa E [Los Alamos National Laboratory

    2010-01-01

    To minimize waste, improve process safety, and minimize costs, modifications were implemented to a method for quantifying gallium in plutonium metal using wavelength dispersive X-ray fluorescence. These changes included reducing sample sizes, reducing ion exchange process volumes, using cheaper reagent grade acids, eliminating the use of HF acid, and using more robust containment film for sample analysis. Relative precision and accuracy achieved from analyzing multiple aliquots from a single parent sample were {approx}0.2% and {approx}0.1% respectively. The same precision was obtained from analyzing a total of four parent materials, and the average relative accuracy from all the samples was 0.4%, which is within programmatic uncertainty requirements.

  20. Visualization of a lost painting by Vincent van Gogh using synchrotron radiation based X-ray fluorescence elemental mapping.

    Science.gov (United States)

    Dik, Joris; Janssens, Koen; Van der Snickt, Geert; van der Loeff, Luuk; Rickers, Karen; Cotte, Marine

    2008-08-15

    Vincent van Gogh (1853-1890), one of the founding fathers of modern painting, is best known for his vivid colors, his vibrant painting style, and his short but highly productive career. His productivity is even higher than generally realized, as many of his known paintings cover a previous composition. This is thought to be the case in one-third of his early period paintings. Van Gogh would often reuse the canvas of an abandoned painting and paint a new or modified composition on top. These hidden paintings offer a unique and intimate insight into the genesis of his works. Yet, current museum-based imaging tools are unable to properly visualize many of these hidden images. We present the first-time use of synchrotron radiation based X-ray fluorescence mapping, applied to visualize a woman's head hidden under the work Patch of Grass by Van Gogh. We recorded decimeter-scale, X-ray fluorescence intensity maps, reflecting the distribution of specific elements in the paint layers. In doing so we succeeded in visualizing the hidden face with unprecedented detail. In particular, the distribution of Hg and Sb in the red and light tones, respectively, enabled an approximate color reconstruction of the flesh tones. This reconstruction proved to be the missing link for the comparison of the hidden face with Van Gogh's known paintings. Our approach literally opens up new vistas in the nondestructive study of hidden paint layers, which applies to the oeuvre of Van Gogh in particular and to old master paintings in general.

  1. Determination of the mass attenuation coefficients for X-ray fluorescence measurements correction by the Rayleigh to Compton scattering ratio

    Energy Technology Data Exchange (ETDEWEB)

    Conti, C.C., E-mail: ccconti@ird.gov.br [Institute for Radioprotection and Dosimetry – IRD/CNEN, Rio de Janeiro (Brazil); Physics Institute, State University of Rio de Janeiro – UERJ, Rio de Janeiro (Brazil); Anjos, M.J. [Physics Institute, State University of Rio de Janeiro – UERJ, Rio de Janeiro (Brazil); Salgado, C.M. [Nuclear Engineering Institute – IEN/CNEN, Rio de Janeiro (Brazil)

    2014-09-15

    Highlights: •This work describes a procedure for sample self-absorption correction. •The use of Monte Carlo simulation to calculate the mass attenuation coefficients curve was effective. •No need for transmission measurement, saving time, financial resources and effort. •This article provides de curves for the 90° scattering angle. •Calculation on-line at (www.macx.net.br). -- Abstract: X-ray fluorescence technique plays an important role in nondestructive analysis nowadays. The development of equipment, including portable ones, enables a wide assortment of possibilities for analysis of stable elements, even in trace concentrations. Nevertheless, despite of the advantages, one important drawback is radiation self-attenuation in the sample being measured, which needs to be considered in the calculation for the proper determination of elemental concentration. The mass attenuation coefficient can be determined by transmission measurement, but, in this case, the sample must be in slab shape geometry and demands two different setups and measurements. The Rayleigh to Compton scattering ratio, determined from the X-ray fluorescence spectrum, provides a link to the mass attenuation coefficient by means of a polynomial type equation. This work presents a way to construct a Rayleigh to Compton scattering ratio versus mass attenuation coefficient curve by using the MCNP5 Monte Carlo computer code. The comparison between the calculated and literature values of the mass attenuation coefficient for some known samples showed to be within 15%. This calculation procedure is available on-line at (www.macx.net.br)

  2. [Rapid determination of major and trace elements in the salt lake clay minerals by X-ray fluorescence spectrometry].

    Science.gov (United States)

    Wang, Xiao-Huan; Meng, Qing-Fen; Dong, Ya-Ping; Chen, Mei-Da; Li, Wu

    2010-03-01

    A rapid multi-element analysis method for clay mineral samples was described. This method utilized a polarized wave-length dispersive X-ray fluorescence spectrometer--Axios PW4400, which had a maximum tube power of 4 000 watts. The method was developed for the determination of As, Mn, Co, Cu, Cr, Dy, Ga, Mo, P, Pb, Rb, S, Sr, Ni, ,Cs, Ta, Th, Ti, U, V, Y, Zn, Zr, MgO, K2O, Na2O, CaO, Fe2O3, Al2O3, SiO2 and so on. Thirty elements in clay mineral species were measured by X-ray fluorescence spectrometry with pressed powder pellets. Spectral interferences, in particular the indirect interferences of each element, were studied. A method to distinguish the interference between each other periodic elements in element periodic table was put forward. The measuring conditions and existence were mainly investigated, and the selected background position as well as corrected spectral overlap for the trace elements were also discussed. It was found that the indirect spectral overlap line was the same important as direct spectral overlap line. Due to inducing the effect of indirect spectral overlap, some elements jlike Bi, Sn, W which do not need analysis were also added to the elements channel. The relative standard deviation (RSD) was in the range of 0.01% to 5.45% except three elements Mo, Cs and Ta. The detection limits, precisions and accuracies for most elements using this method can meet the requirements of sample analysis in clay mineral species.

  3. X-Ray Crystal Structure and Properties of Phanta, a Weakly Fluorescent Photochromic GFP-Like Protein.

    Directory of Open Access Journals (Sweden)

    Craig Don Paul

    Full Text Available Phanta is a reversibly photoswitching chromoprotein (ΦF, 0.003, useful for pcFRET, that was isolated from a mutagenesis screen of the bright green fluorescent eCGP123 (ΦF, 0.8. We have investigated the contribution of substitutions at positions His193, Thr69 and Gln62, individually and in combination, to the optical properties of Phanta. Single amino acid substitutions at position 193 resulted in proteins with very low ΦF, indicating the importance of this position in controlling the fluorescence efficiency of the variant proteins. The substitution Thr69Val in Phanta was important for supressing the formation of a protonated chromophore species observed in some His193 substituted variants, whereas the substitution Gln62Met did not significantly contribute to the useful optical properties of Phanta. X-ray crystal structures for Phanta (2.3 Å, eCGP123T69V (2.0 Å and eCGP123H193Q (2.2 Å in their non-photoswitched state were determined, revealing the presence of a cis-coplanar chromophore. We conclude that changes in the hydrogen-bonding network supporting the cis-chromophore, and its contacts with the surrounding protein matrix, are responsible for the low fluorescence emission of eCGP123 variants containing a His193 substitution.

  4. X-Ray Crystal Structure and Properties of Phanta, a Weakly Fluorescent Photochromic GFP-Like Protein.

    Science.gov (United States)

    Don Paul, Craig; Traore, Daouda A K; Olsen, Seth; Devenish, Rodney J; Close, Devin W; Bell, Toby D M; Bradbury, Andrew; Wilce, Matthew C J; Prescott, Mark

    2015-01-01

    Phanta is a reversibly photoswitching chromoprotein (ΦF, 0.003), useful for pcFRET, that was isolated from a mutagenesis screen of the bright green fluorescent eCGP123 (ΦF, 0.8). We have investigated the contribution of substitutions at positions His193, Thr69 and Gln62, individually and in combination, to the optical properties of Phanta. Single amino acid substitutions at position 193 resulted in proteins with very low ΦF, indicating the importance of this position in controlling the fluorescence efficiency of the variant proteins. The substitution Thr69Val in Phanta was important for supressing the formation of a protonated chromophore species observed in some His193 substituted variants, whereas the substitution Gln62Met did not significantly contribute to the useful optical properties of Phanta. X-ray crystal structures for Phanta (2.3 Å), eCGP123T69V (2.0 Å) and eCGP123H193Q (2.2 Å) in their non-photoswitched state were determined, revealing the presence of a cis-coplanar chromophore. We conclude that changes in the hydrogen-bonding network supporting the cis-chromophore, and its contacts with the surrounding protein matrix, are responsible for the low fluorescence emission of eCGP123 variants containing a His193 substitution.

  5. X-ray instrumentation for analysis of fluorescent and scattered radiation (invited)

    Science.gov (United States)

    Deslattes, Richard D.

    1992-01-01

    Application of high resolution instrumentation to the study of the near-threshold behavior of fluorescent and scattered radiation along with such properties as polarization and angular distribution has proven fertile. This article reviews some alternative strategies for improving the efficiency with which such secondary spectra can be registered.

  6. The Mineralogy of Martian Dust: Design and Analysis Considerations for an X-Ray Diffraction/X-Ray Fluorescence (XRD/XRF) Instrument for Exobiological Studies

    Science.gov (United States)

    Blake, David; Vaniman, David; Bish, David; Morrison, David (Technical Monitor)

    1994-01-01

    A principal objective of Mars exploration is the search for evidence of past life which may have existed during an earlier clement period of Mars history. We would like to investigate the history of surface water activity (which is a requirement for all known forms of life) by identifying and documenting the distribution of minerals which require water for their formation or distribution. A knowledge of the mineralogy of the present Martian surface would help to identify areas which, due to the early activity of water, might have harbored ancient life. It would be desirable to establish the presence and characterize the distribution of hydrated minerals such as clays, and of minerals which are primarily of sedimentary origin such as carbonates, silica and evaporites. Mineralogy, which is more critical to exobiological exploration than is simple chemical analysis (absent the detection of organics), will remain unknown or will at best be imprecisely constrained unless a technique sensitive to mineral structure such as powder X-ray diffraction (XRD) is employed. Additional information is contained in the original extended abstract.

  7. Uranium in surface soils: an easy-and-quick assay combining X-ray diffraction and fluorescence qualitative data

    Science.gov (United States)

    Figueiredo, M. O.; Silva, T. P.; Batista, M. J.; Leote, J.; Ferreira, M. L.; Limpo, V.

    2009-04-01

    Portugal has been a uranium-producer since the beginning of the last century. The uranium-rich area of Alto Alentejo, East-central Portugal, was identified more than fifty years ago [1]. Almost all the uranium-bearing mineralization occurs in schistose rocks of the contact metamorphic aureole produced by intrusion of the Hercynian monzonitic granite of Alto Alentejo into the pre-Ordovitian schist-greywacke complex forming deposits of vein and dissemination type. The Nisa uranium-reservoir, situated at the sharp border of a large and arch shaped granite pluton, was identified in 1957 [2] but its exploitation was considered economically impracticable until recently. However, its existence and the accumulated detritus of these prospect efforts are a concern for local populations [3]. A study of the near-surface soils close to the Nisa reservoir was therefore undertaken to assess the uranium retention by adsorption on clay components under the form of uranyl ions, [UO2]2+ [4-6] and its eventual release into the aquifer groundwater. As an attempt to very quickly appraise the presence of uranium in as-collected near-surface sediment samples a combination of laboratory X-ray techniques was designed: X-ray diffraction (XRD) to identify the mineral phases and roughly estimate its relative proportion plus X-ray fluorescence spectrometry in wavelength dispersive mode (XRF-WDS) to ascertain the presence of uranium and tentatively evaluate its content by comparison with selected chemical components of the soil. A description of the experimental methodology adopted for the implemented easy-and-quick uranium assay is presented. Obtained results compare quite well to the data of certified time-consuming analytical tests of uranium in those soil samples. [1] L. Pilar (1966) Conditions of formation of Nisa uranium deposit (in Portuguese). Comunic. Serv. Geol. Portugal, tomo L, 50-85. [2] C. Gonçalves & J.V. Teixeira Lopes (1971) Uranium deposit of Nisa: geological aspects of its

  8. Multielement analysis of X-Ray fluorescence of Nerium oleander L. Leaves in metropolitan region of Rio de Janeiro

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Ramon S.; Sanches, Francis Anna C.R.A.; Neves, Arthur O.P.; Oliveira, Davi F.; Anjos, Marcelino J., E-mail: ramonziosp@yahoo.com.br, E-mail: francissanches@gmail.com, E-mail: arthur.nevess@yahoo.com.br, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Fisica. Departamento de Fisica Aplicada e Termodinamica

    2015-07-01

    Some plants are used in the detection of the air pollutants due to leaves ability to absorb the pollutants through their stomata and the cuticle, thus, the plants leaves work as a natural sample of the air emissions that are deposited in their self. However, the foliar analysis of these vegetal species can be used to environmental monitoring. The Nerium oleander L. is a specie of plant commonly used as an environmental biomonitor. In this study, Nerium oleander L. leaves were used as biomonitors to evaluate the levels of environmental pollutants in a sub-region in the Metropolitan Region of Rio de Janeiro-Brazil through Energy Dispersive X-ray Fluorescence technique - EDXRF. The EDXRF system was developed in the own laboratory and consist of a portable XRF system formed by a mini X-ray tube of low power (anode of Ag and operated in 15 kV/50 μA and 35 kV/50 μA) and a SiPIN detector. Samples of Nerium oleander L. were collected from adult plants drawn randomly so as not favoring one side of the plant. The samples were collected during the year seasons (summer and winter). It was detected the concentration of 13 elements: S, Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba and Pb, and obtain elemental maps of the regions of study. The study shows that the use of EDXRF technique associated to the Nerium oleander L. leaves used as biomonitor is an efficient, precise, fast and low-cost option for air pollutants analysis. (author)

  9. Study of heavy metals in wild edible mushrooms under different pollution conditions by X-ray fluorescence spectrometry.

    Science.gov (United States)

    Carvalho, M L; Pimentel, A C; Fernandes, B

    2005-07-01

    In this work we studied and compared the metal uptake in edible mushrooms (Lepiota procera, Boletus badius, Boletus edulis, Tricholoma equestry, Lactarius deliciosus, Cantarelus tubalformis and Cantarelus edulis), relative to sampling sites submitted to different pollution conditions: car traffic, soil pollution due to pesticides and fertilizers used in old vineyards, and incineration of hospital waste. Soil was also collected in some places, and its content was correlated to the corresponding one in some mushrooms species. All samples, without any chemical treatment, were analyzed by an X-ray fluorescence set-up. This technique is based on a monochromatic X-ray beam ionizing the atoms of the sample. Following this ionization, the emitted radiation is characteristic of the element, allowing its identification and quantification. Vineyards are normally submitted to very high amounts of sulfating, containing high copper concentrations. This metal is accumulated on the soil, and can be up-taken by vegetation. Very high levels of Fe and Cu were found in Lepiota procera species in old vineyards. Zinc was found to be always higher than Cu by factors ranging from 1.5 to 8 in clean wood taken as a reference for the whole analyzed species, while in old vineyards the ratio Zn/Cu reach 0.25 for Lepiota procera. This is correlated to the soil content for both elements. In addition, pollution induced by car traffic was checked in some samples, collected in the proximity of highways. Pb was the main contaminant in these areas, and presenting values 10 times higher than the corresponding ones in sites not submitted to pollution, for some species. Mushrooms contamination due to incineration of hospital waste was also studied, but we did not observe any contamination involving heavy metals in the several analyzed species around these areas. This is in agreement with what was expected, taking into account that hospital waste is mostly organic and, in principle, no heavy metals would

  10. TU-A-9A-05: First Experimental Demonstration of the Anisotropic Detection Principle in X-Ray Fluorescence Computed Tomography

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, M; Bazalova, M; Fahrig, R; Xing, L [Stanford University, Stanford, CA (United States)

    2014-06-15

    Purpose: To improve the sensitivity of X-ray fluorescence computed tomography (XFCT) for in vivo molecular imaging. Is the maximum sensitivity achieved with an isotropic (4π) detector configuration? We prove that this is not necessarily true, and that a greater sensitivity is possible with anisotropic detector configuration. Methods: An XFCT imaging system was constructed consisting of 1) a collimated pencil beam x-ray source using a fluoroscopy grade x-ray tube; 2) a CdTe x-ray photon counting detector to detect fluorescent x-rays; and 3) a rotation/translation stage for tomographic imaging. We created a 6.5-cm diameter water phantom with 2-cm inserts of low gold concentration (0.25%–1%) to simulate tumors targeted by gold nano-particles. The placement of x-ray fluorescence detector were chosen to minimize scatter x-rays. XFCT imaging was performed at three different detector positions (60°, 90°, 145°) to determine the impact of forward-scatter, side-scatter, and back-scatter on imaging performance. The three data sets were also combined to estimate the imaging performance with an isotropic detector. Results: The highest imaging performance was achieved when the XF detector was in the backscatter 145° configuration. The signal-to-noise ratio (SNR) was 5.5 for the 0.25% gold concentration compared to SNRs of 1.4, 0, and 2.4 for 60°, 90°, and combined (60°+90°+145°) datasets. Only the 145° detector arrangement alone could detect the 0.25% concentration. The imaging dose was 14 mGy for each detector arrangement experiment. Conclusion: This study experimentally proves, for the fist time, the Anisotropic Detection Principle in XF imaging, which holds that optimized anisotropic x-ray fluorescence detection provides greater sensitivity than isotropic detection. The optimized detection arrangement was used to improve the sensitivity of the XFCT experiment. The achieved XFCT sensitivity is the highest ever for a phantom at least this large using a benchtop x-ray

  11. JGIXA - A software package for the calculation and fitting of grazing incidence X-ray fluorescence and X-ray reflectivity data for the characterization of nanometer-layers and ultra-shallow-implants

    Science.gov (United States)

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

    2016-04-01

    Grazing incidence XRF (GIXRF) is a very surface sensitive, nondestructive analytical tool making use of the phenomenon of total external reflection of X-rays on smooth polished surfaces. In recent years the method experienced a revival, being a powerful tool for process analysis and control in the fabrication of semiconductor based devices. Due to the downscaling of the process size for semiconductor devices, junction depths as well as layer thicknesses are reduced to a few nanometers, i.e. the length scale where GIXRF is highly sensitive. GIXRF measures the X-ray fluorescence induced by an X-ray beam incident under varying grazing angles and results in angle dependent intensity curves. These curves are correlated to the layer thickness, depth distribution and mass density of the elements in the sample. But the evaluation of these measurements is ambiguous with regard to the exact distribution function for the implants as well as for the thickness and density of nanometer-thin layers. In order to overcome this ambiguity, GIXRF can be combined with X-ray reflectometry (XRR). This is straightforward, as both techniques use similar measurement procedures and the same fundamental physical principles can be used for a combined data evaluation strategy. Such a combined analysis removes ambiguities in the determined physical properties of the studied sample and, being a correlative spectroscopic method, also significantly reduces experimental uncertainties of the individual techniques. In this paper we report our approach to a correlative data analysis, based on a concurrent calculation and fitting of simultaneously recorded GIXRF and XRR data. Based on this approach we developed JGIXA (Java Grazing Incidence X-ray Analysis), a multi-platform software package equipped with a user-friendly graphic user interface (GUI) and offering various optimization algorithms. Software and data evaluation approach were benchmarked by characterizing metal and metal oxide layers on

  12. Elemental analysis of human amniotic fluid and placenta by total-reflection X-ray fluorescence and energy-dispersive X-ray fluorescence: child weight and maternal age dependence

    Science.gov (United States)

    Carvalho, M. L.; Custódio, P. J.; Reus, U.; Prange, A.

    2001-11-01

    This work is an attempt to evaluate the possible influence of the mother's age in trace element concentrations in human amniotic fluid and placenta and whether these concentrations are correlated to the weight of the newborn infants. Total-reflection X-ray fluorescence (TXRF) was used to analyze 16 amniotic fluid samples, and the placenta samples were analyzed by energy dispersive X-ray fluorescence (EDXRF). The whole samples were collected during delivery from healthy mothers and healthy infants and full-term pregnancies. According to the age of the mother, three different groups were considered: 20-25, 25-30 and 30-40 years old. Only two mothers were aged more than 35 years. The weight of the infants ranged from 2.56 to 4.05 kg and three groups were also considered: 2.5-3, 3-3.5 and 3.5-4 kg. The organic matrix of the amniotic fluid samples was removed by treatment with HNO 3 followed by oxygen plasma ashing. Yttrium was used as the internal standard for TXRF analysis. Placenta samples were lyophilized and analyzed by EDXRF without any chemical treatment. Very low levels of Ni and Sr were found in the amniotic fluid samples, and were independent of the age of the mother and weight of the child. Cr, Mn, Se and Pb were at the level of the detection limit. Zn, considered one of the key elements in neonatal health, was not significantly different in the samples analyzed; however, it was weakly related to birth weigh. The concentrations obtained ranged from 0.11 to 0.92 mg/l and 30 to 65 μg/g in amniotic fluid and placenta, respectively. The only two elements which seemed to be significantly correlated with mother's age and newborn weight were Ca and Fe for both types of sample: Ca levels were increased in heavier children and older mothers; however, Fe increased with increasing maternal age, but decreased for heavier babies. The same conclusions were obtained for placenta and amniotic fluid samples. Cu is closely associated with Fe in its function in the organism

  13. Element distribution and iron speciation in mature wheat grains (Triticum aestivum L.) using synchrotron X-ray fluorescence microscopy mapping and X-ray absorption near-edge structure (XANES) imaging.

    Science.gov (United States)

    De Brier, Niels; Gomand, Sara V; Donner, Erica; Paterson, David; Smolders, Erik; Delcour, Jan A; Lombi, Enzo

    2016-08-01

    Several studies have suggested that the majority of iron (Fe) and zinc (Zn) in wheat grains are associated with phytate, but a nuanced approach to unravel important tissue-level variation in element speciation within the grain is lacking. Here, we present spatially resolved Fe-speciation data obtained directly from different grain tissues using the newly developed synchrotron-based technique of X-ray absorption near-edge spectroscopy imaging, coupling this with high-definition μ-X-ray fluorescence microscopy to map the co-localization of essential elements. In the aleurone, phosphorus (P) is co-localized with Fe and Zn, and X-ray absorption near-edge structure imaging confirmed that Fe is chelated by phytate in this tissue layer. In the crease tissues, Zn is also positively related to P distribution, albeit less so than in the aleurone. Speciation analysis suggests that Fe is bound to nicotianamine rather than phytate in the nucellar projection, and that more complex Fe structures may also be present. In the embryo, high Zn concentrations are present in the root and shoot primordium, co-occurring with sulfur and presumably bound to thiol groups. Overall, Fe is mainly concentrated in the scutellum and co-localized with P. This high resolution imaging and speciation analysis reveals the complexity of the physiological processes responsible for element accumulation and bioaccessibility.

  14. A turn-on fluorescent chemosensor for Zn2+ ion: X-ray structure and application in cell imaging study

    Science.gov (United States)

    Ghosh, Koushik; Dey, Sudipto; Halder, Shibashis; Bhattacharjee, Aradhita; Rizzoli, Corrado; Roy, Partha

    2016-08-01

    The selective fluorescence zinc(II) sensing properties of a Schiff-base compound, 2-methoxy-6-(2-morpholinoethyliminomethyl)phenol (HL) have been explored. The emission intensity of HL in the presence of one equivalent of Zn2+ ion increases by about 25 times. Several other metal ions, except Cd2+ and Ni2+, have not been able to increase the emission intensity of HL significantly. The quantum yield and life-time of HL have also been increased in the presence of Zn2+ ions. The enhancement in fluorescence intensity of HL is mainly due to the restriction of ESIPT, CHEF and PET on complex formation. HL forms a complex with Zn2+ in 1:1 ratio as evidenced by Job's plot analysis and X-ray single crystal structure determination. Some theoretical calculations have been performed to get a better view on the nature of the observed electronic transitions. The probe has been applied for imaging of DLD-1, human colorectal adenocarcinoma cell.

  15. L X-ray fluorescence cross sections experimentally determined for elements with 45

    Energy Technology Data Exchange (ETDEWEB)

    Bonzi, Edgardo V., E-mail: bonzie@famaf.unc.edu.ar [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, Ciudad Universitaria-5010, Cordoba (Argentina); Badiger, Nagappa M. [Departments of Physics, Karnatak University, Dharwad 580 003, Karnataka (India); Grad, Gabriela B. [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, Ciudad Universitaria-5010, Cordoba (Argentina); Barrea, Raul A. [The Biophysics Collaborative Access Team (BioCAT), Dept of Biological Chemical, and Physical Sciences, Illinois Institute of Technology, Chicago, IL 60616 (United States); Figueroa, Rodolo G. [Departamento de Cs. Fisicas, Universidad de La Frontera, Temuco (Chile)

    2012-04-15

    Experimental determination of L fluorescence cross-sections for elements with 45X-ray photons, Ll, L{alpha}, L{beta}{sub I}, L{beta}{sub II}, L{gamma}{sub {Iota}} and L{gamma}{sub {Iota}{Iota}} produced in the target were measured using a Si(Li) detector. The experimental set-up provided a low background by using linearly polarized monoenergetic photon beam, improving the signal-to-noise ratio. The experimental cross sections obtained in this work were compared with data calculated using coefficients from , , and Scofield and Puri et al. (1993, 1995) - Highlights: Black-Right-Pointing-Pointer Experimental data of L fluorescence cross-sections with 45

  16. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence

    Energy Technology Data Exchange (ETDEWEB)

    Wobrauschek, P., E-mail: wobi@ati.ac.at; Prost, J.; Ingerle, D.; Kregsamer, P.; Streli, C. [Atominstitut, TU Wien, Stadionallee 2, 1020 Vienna (Austria); Misra, N. L. [Fuel Chemistry Division, Bhabha Atomic Research Centre (BARC), Mumbai 400085 (India)

    2015-08-15

    The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm{sup 2} active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.

  17. The determination of major and some minor constituents in lead zirconate-titanate compositions by x-ray fluorescence and atomic absorption spectrometry

    NARCIS (Netherlands)

    Willigen, van J.H.H.G.; Kruidhof, H.; Dahmen, E.A.M.F.

    1972-01-01

    An accurate X-ray fluorescence spectrometric method is described for the determination of lead, zirconium and titanium in lead zirconate-titanate ceramics. Careful matching of samples and standards by a borax fusion method resulted in a relative standard deviation of about 0.2% for the major constit

  18. Applicability of X-ray fluorescence spectroscopy as method to determine thickness and composition of stacks of metal thin films: A comparison with imaging and profilometry

    NARCIS (Netherlands)

    Vrielink, J.A.M.; Tiggelaar, R.M.; Gardeniers, J.G.E.; Lefferts, L.

    2012-01-01

    In this work the applicability of X-ray fluorescence spectroscopy (XRF) for fast, accurate and non-destructive determination of the thickness of a variety of single-layer and multi-layer metal thin films deposited on glass and silicon is investigated. Data obtained with XRF is compared with informat

  19. Trace elements as tumor biomarkers and prognostic factors in breast cancer: a study through energy dispersive x-ray fluorescence

    Directory of Open Access Journals (Sweden)

    Silva Marina P

    2012-07-01

    Full Text Available Abstract Background The application and better understanding of traditional and new breast tumor biomarkers and prognostic factors are increasing due to the fact that they are able to identify individuals at high risk of breast cancer, who may benefit from preventive interventions. Also, biomarkers can make possible for physicians to design an individualized treatment for each patient. Previous studies showed that trace elements (TEs determined by X-Ray Fluorescence (XRF techniques are found in significantly higher concentrations in neoplastic breast tissues (malignant and benign when compared with normal tissues. The aim of this work was to evaluate the potential of TEs, determined by the use of the Energy Dispersive X-Ray Fluorescence (EDXRF technique, as biomarkers and prognostic factors in breast cancer. Methods By using EDXRF, we determined Ca, Fe, Cu, and Zn trace elements concentrations in 106 samples of normal and breast cancer tissues. Cut-off values for each TE were determined through Receiver Operating Characteristic (ROC analysis from the TEs distributions. These values were used to set the positive or negative expression. This expression was subsequently correlated with clinical prognostic factors through Fisher’s exact test and chi-square test. Kaplan Meier survival curves were also evaluated to assess the effect of the expression of TEs in the overall patient survival. Results Concentrations of TEs are higher in neoplastic tissues (malignant and benign when compared with normal tissues. Results from ROC analysis showed that TEs can be considered a tumor biomarker because, after establishing a cut-off value, it was possible to classify different tissues as normal or neoplastic, as well as different types of cancer. The expression of TEs was found statistically correlated with age and menstrual status. The survival curves estimated by the Kaplan-Meier method showed that patients with positive expression for Cu presented a poor

  20. X-ray fluorescence analysis with micro glass beads using milligram-scale siliceous samples for archeology and geochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Ichikawa, Shintaro, E-mail: sichi@meiji.ac.jp [Organization for the Strategic Coordination of Research and Intellectual Properties, Meiji University, Kawasaki 214-8571 (Japan); Nakamura, Toshihiro [Department of Applied Chemistry, Meiji University, Kawasaki 214-8571 (Japan)

    2014-06-01

    A micro glass bead technique was developed to assay precious siliceous samples for geochemical and archeological analyses. The micro-sized (approximately 3.5 mm in diameter and 0.8 mm in height) glass beads were prepared by mixing and fusing 1.1 mg of the powdered sample and 11.0 mg of the alkali lithium tetraborate flux for wavelength-dispersive X-ray fluorescence determination of major oxides (Na{sub 2}O, MgO, Al{sub 2}O{sub 3}, SiO{sub 2}, P{sub 2}O{sub 5}, K{sub 2}O, CaO, TiO{sub 2}, MnO, and total Fe{sub 2}O{sub 3}). The preparation parameters, including temperature and agitation during the fusing process, were optimized for the use of a commercial platinum crucible rather than a custom-made crucible. The procedure allows preparation of minute sample amounts of siliceous samples using conventional fusing equipment. Synthetic calibration standards were prepared by compounding chemical reagents such as oxides, carbonates, and diphosphates. Calibration curves showed good linearity with r values > 0.997, and the lower limits of detection were in the 10s to 100s of μg g{sup −1} range (e.g., 140 μg g{sup −1} for Na{sub 2}O, 31 μg g{sup −1} for Al{sub 2}O{sub 3}, and 8.9 μg g{sup −1} for MnO). Using the present method, we determined ten major oxides in igneous rocks, stream sediments, ancient potteries, and obsidian. This was applicable to siliceous samples with various compositions, because of the excellent agreement between the analytical and recommended values of six geochemical references. This minimal-scale analysis may be available for precious and limited siliceous samples (e.g., rock, sand, soil, sediment, clay, and archeological ceramics) in many fields such as archeology and geochemistry. - Highlights: • X-ray fluorescence determination of major oxides was performed using 1.1 mg of sample. • Preparation and measurement techniques of the XRF micro glass bead specimen were optimized. • Calibration curves using synthetic standards showed good

  1. X-Ray Fluorescence Spectrometry. II Determination of Uranium in ores; Espectrometria de fluorescencia de Rayos X. II-Aplicacion a la determinacion de uranio en minerales

    Energy Technology Data Exchange (ETDEWEB)

    Bermudez Polonio, J.; Crus Castillo, F. de la; Fernandez Cellini, R.

    1961-07-01

    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 {alpha}{sub 1} spectral line is calculated and related to corresponding strontium-K{sub {alpha}} spectral line, both detected with a Scintillation Counter. (Author) 31 refs.

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

    Energy Technology Data Exchange (ETDEWEB)

    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); Van Pevenage, Jolien [Ghent University, Department of Analytical Chemistry, Raman Spectroscopy Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); De Langhe, Kaat [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo [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); Martens, Maximiliaan P.J. [Ghent University, Department of Art, Music and Theatre Sciences, Blandijnberg 2, B-9000 Gent (Belgium)

    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% SiO{sub 2} + 15% K{sub 2}O + 10% CoO + 5% Al{sub 2}O{sub 3}) 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. - Highlights: • In situ, non-destructive investigation of a famous painting by Pieter Bruegel. • Use of a new, commercial available, portable XRF/XRD instrumentation. • Multi-methodological approach: make also use of a mobile Raman spectrometer. • Used pigments and different preparation layers of the painting are characterized. • The verification of two important historical iconographic hypotheses are performed.

  3. Manganese accumulates within golgi apparatus in dopaminergic cells as revealed by synchrotron X-ray fluorescence nanoimaging.

    Science.gov (United States)

    Carmona, Asunción; Devès, Guillaume; Roudeau, Stéphane; Cloetens, Peter; Bohic, Sylvain; Ortega, Richard

    2010-03-17

    Chronic exposure to manganese results in neurological symptoms referred to as manganism and is identified as a risk factor for Parkinson's disease. In vitro, manganese induces cell death in the dopaminergic cells, but the mechanisms of manganese cytotoxicity are still unexplained. In particular, the subcellular distribution of manganese and its interaction with other trace elements needed to be assessed. Applying synchrotron X-ray fluorescence nanoimaging, we found that manganese was located within the Golgi apparatus of PC12 dopaminergic cells at physiologic concentrations. At increasing concentrations, manganese accumulates within the Golgi apparatus until cytotoxic concentrations are reached resulting in a higher cytoplasmic content probably after the Golgi apparatus storage capacity is exceeded. Cell exposure to manganese and brefeldin A, a molecule known to specifically cause the collapse of the Golgi apparatus, results in the striking intracellular redistribution of manganese, which accumulates in the cytoplasm and the nucleus. These results indicate that the Golgi apparatus plays an important role in the cellular detoxification of manganese. In addition manganese exposure induces a decrease in total iron content, which could contribute to the overall neurotoxicity.

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

    Energy Technology Data Exchange (ETDEWEB)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia (COPPE). Nuclear Instrumentation Lab.]. E-mail: renata@lin.ufrj.br; Anjos, Marcelino J. dos [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Physics Inst.]. E-mail: marcelin@lin.ufrj.br; Carmo, Maria G.T. do [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Nutrition Inst.; Rocha, Monica S. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Dept. of Basics and Clinic Pharmacy; Moreira, Silvana [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Civil Engineering Dept.; Martinez, Ana M.B. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Dept. of Histology and Embryology

    2007-07-01

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

  5. [X-ray fluorescence spectrum analysis of chemical element for spider and silkworm silk and its applications].

    Science.gov (United States)

    Yuan, Bo; Xu, Ze-ren; Xie, Zhuo-jun; Shi, Qiang; Zhang, Xing-kang; Xu, Si-chuan

    2010-07-01

    Elemental compositions in spider and silkworm silks were determined by X-ray fluorescence (XRF) spectrum to probe the silk-forming mechanisms and an elemental basis for spider silk with excellent characteristics. XRF analysis demonstrates that in the silkworm silk, the elemental content is 47.10% for C, 29.92% for O and 16. 52% for N, including metal elemental contents: 0.166 2% for Ca, 0.104 0% for Mg and 0.039 5% for K, while Na, Zn, Ni, Fe and Cr show less micro quantity. Due to relative high quantity for Ca and Mg, they both play an important role in the silk-forming mechanism by silkworm. In the spider silk, the determined main nonmetal elemental contents are 44.09% for C, 26.64% for O and 22.34% for N. The high content of nitrogen may be an elemental basis for spider silk with excellent characteristic. The main metal elemental contents are 0.268 0% for Na, 0.081 4% for K and 0.011 6% for Mg, while Ca, Zn, Ni, Cu and Cr possess less micro quantity in the spider silk. Because of relative high quantity for Na and K, they both play an important role in the silk-forming mechanism by spider. The elemental compositions investigated by using mathematic statistic method are quite in agreement with those demonstrated by using XRF spectrum, which validates the experimentally determined elemental compositions in the spider and silkworm silks.

  6. Simultaneous nondestructive analysis of palladium, rhodium, platinum, and gold nanoparticles using energy dispersive X-ray fluorescence.

    Science.gov (United States)

    Fiedler, Haidi D; Drinkel, Emma E; Orzechovicz, Beatriz; Leopoldino, Elder C; Souza, Franciane D; Almerindo, Gizelle I; Perdona, Cristian; Nome, Faruk

    2013-11-01

    A selective method is proposed for the determination of palladium, gold, and sulfur in catalytic systems, by direct liquid analysis using energy dispersive X-ray fluorescence (EDXRF), under an atmosphere of helium or air. This method allows a nondestructive analysis of palladium, rhodium, platinum, and gold nanoparticulate catalysts stabilized by imidazolium propane sulfonate based zwitterionic surfactants, allowing the samples to be reused for catalytic studies. The signals from palladium, rhodium, platinum, and gold samples in the presence of imidazolium propane sulfonate-based zwitterionic surfactants obtained using EDXRF before (Pd(2+), Rh(2+), Pt(2+), and Au(3+)) and after (Pd(0), Rh(0), Pt(0), and Au(0)) formation of nanoparticles are essentially identical. The results show that the EDXRF method is nondestructive and allows detection and quantification of the main components of platinum, gold, rhodium, and palladium NPs, including the surfactant concentration, with detection and quantification limits in the range of 0.4-3 mg L(-1). The matrices used in such samples present no problems, even allowing the detection and quantification of interfering elements.

  7. Characterization of uranium bearing material using x-ray fluorescence and direct gamma-rays measurement techniques

    Energy Technology Data Exchange (ETDEWEB)

    Mujaini, M., E-mail: madihah@uniten.edu.my; Chankow, N. [Faculty of Engineering, Chulalongkorn University Phyathai Rd., Wang Mai, Patumwan, Bangkok 10330 (Thailand); Yusoff, M. Z.; Hamid, N. A. [College of Engineering, Universiti Tenaga Nasional 43000 Kajang, Selangor (Malaysia)

    2016-01-22

    Uranium ore can be easily detected due to various gamma-ray energies emitted from uranium daughters particularly from {sup 238}U daughters such as {sup 214}Bi, {sup 214}Pb and {sup 226}Ra. After uranium is extracted from uranium ore, only low energy gamma-rays emitted from {sup 235}U may be detected if the detector is placed in close contact to the specimen. In this research, identification and characterization of uranium bearing materials is experimentally investigated using direct measurement of gamma-rays from {sup 235}U in combination with the x-ray fluorescence (XRF) technique. Measurement of gamma-rays can be conducted by using high purity germanium (HPGe) detector or cadmium telluride (CdTe) detector while a {sup 57}Coradioisotope-excited XRF spectrometer using CdTe detector is used for elemental analysis. The proposed technique was tested with various uranium bearing specimens containing natural, depleted and enriched uranium in both metallic and powder forms.

  8. Synchrotron-based X-ray fluorescence microscopy enables multiscale spatial visualization of ions involved in fungal lignocellulose deconstruction

    Science.gov (United States)

    Kirker, Grant; Zelinka, Sam; Gleber, Sophie-Charlotte; Vine, David; Finney, Lydia; Chen, Si; Hong, Young Pyo; Uyarte, Omar; Vogt, Stefan; Jellison, Jody; Goodell, Barry; Jakes, Joseph E.

    2017-01-01

    The role of ions in the fungal decay process of lignocellulose biomaterials, and more broadly fungal metabolism, has implications for diverse research disciplines ranging from plant pathology and forest ecology, to carbon sequestration. Despite the importance of ions in fungal decay mechanisms, the spatial distribution and quantification of ions in lignocellulosic cell walls and fungal hyphae during decay is not known. Here we employ synchrotron-based X-ray fluorescence microscopy (XFM) to map and quantify physiologically relevant ions, such as K, Ca, Mn, Fe, and Zn, in wood being decayed by the model brown rot fungus Serpula lacrymans. Two-dimensional XFM maps were obtained to study the ion spatial distributions from mm to submicron length scales in wood, fungal hyphae with the dried extracellular matrix (ECM) from the fungus, and Ca oxalate crystals. Three-dimensional ion volume reconstructions were also acquired of wood cell walls and hyphae with ECM. Results show that the fungus actively transports some ions, such as Fe, into the wood and controls the distribution of ions at both the bulk wood and cell wall length scales. These measurements provide new insights into the movement of ions during decay and illustrate how synchrotron-based XFM is uniquely suited study these ions. PMID:28139778

  9. Determination of heavy metals in macrozoobenthos from the rivers Tisza and Szamos by total reflection X-ray fluorescence spectrometry

    Science.gov (United States)

    Woelfl, S.; Mages, M.; Óvári, M.; Geller, W.

    2006-11-01

    In 2000, accidents in the Romanian mining industry in key catchment areas led to heavy metal contamination of the Hungarian rivers Tisza and Szamos resulting in substantial heavy metal loads in several sediments of the upper river basins. This enhanced metal content might have been bioaccumulated in benthic organisms during the following years. Therefore, the aim of this study was to test, whether the zoobenthic fauna showed an enhanced metal content 3 years after the industrial accident. Macrozoobenthic insect larvae (chironomids) were sampled 100 m below and above the confluent site of the rivers Tisza and Szamos during summer 2003 and for comparison purpose also in the river Maros, a tributary of the Tisza river, during 2005. In order to determine their heavy metal content, single specimens were prepared and analysed by Total Reflection X-ray Fluorescence Spectrometry (TRXF) according to the modified dry method. Fe was much lower and Mn and Zn much higher concentrated in benthos from the more contaminated Szamos river compared to the Tisza and Maros rivers. In this sense, the benthic organisms reflected very well the enhanced metal concentrations in the contaminated rivers being suitable as bioindicators of metal contamination. However, the sediment bioaccumulation factor was low at all sampling sites indicating a low bioavailability of trace metals for benthic organisms.

  10. Synchrotron-based X-ray fluorescence microscopy enables multiscale spatial visualization of ions involved in fungal lignocellulose deconstruction

    Science.gov (United States)

    Kirker, Grant; Zelinka, Sam; Gleber, Sophie-Charlotte; Vine, David; Finney, Lydia; Chen, Si; Hong, Young Pyo; Uyarte, Omar; Vogt, Stefan; Jellison, Jody; Goodell, Barry; Jakes, Joseph E.

    2017-01-01

    The role of ions in the fungal decay process of lignocellulose biomaterials, and more broadly fungal metabolism, has implications for diverse research disciplines ranging from plant pathology and forest ecology, to carbon sequestration. Despite the importance of ions in fungal decay mechanisms, the spatial distribution and quantification of ions in lignocellulosic cell walls and fungal hyphae during decay is not known. Here we employ synchrotron-based X-ray fluorescence microscopy (XFM) to map and quantify physiologically relevant ions, such as K, Ca, Mn, Fe, and Zn, in wood being decayed by the model brown rot fungus Serpula lacrymans. Two-dimensional XFM maps were obtained to study the ion spatial distributions from mm to submicron length scales in wood, fungal hyphae with the dried extracellular matrix (ECM) from the fungus, and Ca oxalate crystals. Three-dimensional ion volume reconstructions were also acquired of wood cell walls and hyphae with ECM. Results show that the fungus actively transports some ions, such as Fe, into the wood and controls the distribution of ions at both the bulk wood and cell wall length scales. These measurements provide new insights into the movement of ions during decay and illustrate how synchrotron-based XFM is uniquely suited study these ions.

  11. Determination of heavy metals in macrozoobenthos from the rivers Tisza and Szamos by total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woelfl, S. [Universidad Austral de Chile, Instituto de Zoologia, Casilla 567, Valdivia (Chile)]. E-mail: swoelfl@uach.cl; Mages, M. [Helmhotz Centre for Environmental Research (UFZ), Department of River Ecology, Brueckstrasse 3a, D-39114, Magdeburg (Germany); Ovari, M. [Ovari, M. Eoetvoes University, Department of Organic Chemistry, H-1117, Budapest, Pazmany P. stny. 1/a (Hungary); Geller, W. [Helmhotz Centre for Environmental Research (UFZ), Department of River Ecology, Brueckstrasse 3a, D-39114, Magdeburg (Germany)

    2006-11-15

    In 2000, accidents in the Romanian mining industry in key catchment areas led to heavy metal contamination of the Hungarian rivers Tisza and Szamos resulting in substantial heavy metal loads in several sediments of the upper river basins. This enhanced metal content might have been bioaccumulated in benthic organisms during the following years. Therefore, the aim of this study was to test, whether the zoobenthic fauna showed an enhanced metal content 3 years after the industrial accident. Macrozoobenthic insect larvae (chironomids) were sampled 100 m below and above the confluent site of the rivers Tisza and Szamos during summer 2003 and for comparison purpose also in the river Maros, a tributary of the Tisza river, during 2005. In order to determine their heavy metal content, single specimens were prepared and analysed by Total Reflection X-ray Fluorescence Spectrometry (TRXF) according to the modified dry method. Fe was much lower and Mn and Zn much higher concentrated in benthos from the more contaminated Szamos river compared to the Tisza and Maros rivers. In this sense, the benthic organisms reflected very well the enhanced metal concentrations in the contaminated rivers being suitable as bioindicators of metal contamination. However, the sediment bioaccumulation factor was low at all sampling sites indicating a low bioavailability of trace metals for benthic organisms.

  12. Distribution of toxic elements in teeth treated with amalgam using μ-energy dispersive X-ray fluorescence

    Science.gov (United States)

    Guerra, M.; Ferreira, C.; Carvalho, M. L.; Santos, J. P.; Pessanha, S.

    2016-08-01

    Over the years, the presence of mercury in amalgam fillings has raised some safety concerns. Amalgam is one of the most commonly used tooth fillings and contains approximately 50% of elemental mercury and 50% of other metals, mostly silver, tin and copper. Amalgam can release small amounts of mercury vapor over time, and patients can absorb these vapors by inhaling or ingesting them. In this study, 10 human teeth treated with dental amalgam were analyzed using energy dispersive X-ray fluorescence (EDXRF) to study the diffusion of its constituents, Ag, Cu, Sn and Hg. The used EDXRF setup, makes use of a polycapillary lens to focus radiation up to 25 μm allowing the mapping of the elemental distribution in the samples. Quantification was performed using the inbuilt software based on the Fundamental Parameters method for bulk samples, considering a hydroxyapatite matrix. The teeth were longitudinally cut and each slice was scanned from the surface enamel to the inner region (dentin and pulp cavity). Mercury concentration profiles show strong levels of this element close to the amalgam region, decreasing significantly in the dentin, and increasing again up to 40,000 μg·g- 1 in the cavity were the pulp used to exist when the tooth was vital.

  13. Analytical capabilities of total reflection X-ray fluorescence spectrometry for silver nanoparticles determination in soil adsorption studies

    Science.gov (United States)

    Torrent, Laura; Iglesias, Mònica; Hidalgo, Manuela; Marguí, Eva

    2016-12-01

    In recent years, the production of silver nanoparticles (AgNPs) has grown due to their antibacterial properties. This fact enhances the release of these particles into the environment, especially in soils that are the major sink. To better understand adsorption processes in soils, usually batch kinetic studies are carried out. In this context, we tested the possibilities of using total reflection X-ray fluorescence spectrometry (TXRF) to monitor the silver content in soil adsorption kinetic studies. It was found that the lower limit of detection for Ag (through Ag-Kα detection) in aqueous solutions was around 37 μg·L- 1, which was suitable to carry out this kind of studies. Moreover, the direct analysis of Ag adsorbed onto soil after the kinetic studies was investigated. In this case, the limit of detection for Ag was around 1.7 mg·kg- 1. All TXRF results were compared with those obtained by inductively coupled plasma optic emission spectrometry and good agreement was found. The batch adsorption tests performed showed that 98% of polyvinylpyrrolidone coated AgNPs were retained on the tested soils in < 6 h.

  14. Standard test method for determination of low concentrations of uranium in oils and organic liquids by X-ray fluorescence

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of oils and organic solutions containing uranium. Two different preparation techniques are described. 1.2 The procedure is valid for those solutions containing 20 to 2000 μg uranium per mL as presented to the spectrometer for the solution technique and 200 to 50 000 μg uranium per g for the pellet technique. 1.3 This test method requires the use of an appropriate internal standard. Care must be taken to ascertain that samples analyzed by this test method do not contain the internal standard or that this contamination, whenever present, has been corrected for mathematically. Such corrections are not addressed in this procedure. Care must be taken that the internal standard and sample medium are compatible; that is, samples must be miscible with tri-n-butyl phosphate (TBP) and must not remove the internal standard from solution. Alternatively, a scatter line may be used as the internal standard. 1....

  15. A new methodology for measurement of sludge residence time distribution in a paddle dryer using X-ray fluorescence analysis.

    Science.gov (United States)

    Charlou, Christophe; Milhé, Mathieu; Sauceau, Martial; Arlabosse, Patricia

    2015-02-01

    Drying is a necessary step before sewage sludge energetic valorization. Paddle dryers allow working with such a complex material. However, little is known about sludge flow in this kind of processes. This study intends to set up an original methodology for sludge residence time distribution (RTD) measurement in a continuous paddle dryer, based on the detection of mineral tracers by X-ray fluorescence. This accurate analytical technique offers a linear response to tracer concentration in dry sludge; the protocol leads to a good repeatability of RTD measurements. Its equivalence to RTD measurement by NaCl conductivity in sludge leachates is assessed. Moreover, it is shown that tracer solubility has no influence on RTD: liquid and solid phases have the same flow pattern. The application of this technique on sludge with different storage duration at 4 °C emphasizes the influence of this parameter on sludge RTD, and thus on paddle dryer performances: the mean residence time in a paddle dryer is almost doubled between 24 and 48 h of storage for identical operating conditions.

  16. Determination of Te, Bi, Ni, Sb and Au by X-ray fluorescence spectrometry following electroenrichment on a copper cathode

    Science.gov (United States)

    Zawisza, Beata; Sitko, Rafał

    2007-10-01

    The electrodepositons of Te, Bi, Ni, Sb and Au from aqueous solution of pH = 1 on the cathode surface have been studied for X-ray fluorescence analysis (XRF). A special holder for a copper electrode has been constructed to perform the electrodeposition process on only one side of the electrode. After electrolysis, the copper electrode can be easily removed from the holder; after rinsing it with water and drying it can be analyzed by XRF. The proposed method of sample preparation and preconcentration of Te, Bi, Ni, Sb, Au provides suitable samples which are devoid of the negative and undesirable effects of XRF analysis, such as particle size and matrix effects. The influence of time on the deposition yield has been examined. The method of preconcentration is efficient. The inhomogeneity of the prepared specimens has been studied using internal standard method. The calibration is based on using synthetic standards, certified reference materials and standard addition method. The best results are achieved by the standard addition method. The agreement between results obtained with XRF analysis and certified values is satisfactory and indicates the usefulness of the proposed method for determination of Te, Bi, Ni, Sb and Au in anode slime.

  17. Standard test method for analysis of uranium and thorium in soils by energy dispersive X-Ray fluorescence spectroscopy

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the energy dispersive X-ray fluorescence (EDXRF) spectrochemical analysis of trace levels of uranium and thorium in soils. Any sample matrix that differs from the general ground soil composition used for calibration (that is, fertilizer or a sample of mostly rock) would have to be calibrated separately to determine the effect of the different matrix composition. 1.2 The analysis is performed after an initial drying and grinding of the sample, and the results are reported on a dry basis. The sample preparation technique used incorporates into the sample any rocks and organic material present in the soil. This test method of sample preparation differs from other techniques that involve tumbling and sieving the sample. 1.3 Linear calibration is performed over a concentration range from 20 to 1000 μg per gram for uranium and thorium. 1.4 The values stated in SI units are to be regarded as the standard. The inch-pound units in parentheses are for information only. 1.5 This standard...

  18. Wavelength dispersive X-ray fluorescence analysis using fundamental parameter approach of Catha edulis and other related plant samples

    Science.gov (United States)

    Shaltout, Abdallah A.; Moharram, Mohammed A.; Mostafa, Nasser Y.

    2012-01-01

    This work is the first attempt to quantify trace elements in the Catha edulis plant (Khat) with a fundamental parameter approach. C. edulis is a famous drug plant in east Africa and Arabian Peninsula. We have previously confirmed that hydroxyapatite represents one of the main inorganic compounds in the leaves and stalks of C. edulis. Comparable plant leaves from basil, mint and green tea were included in the present investigation as well as trifolium leaves were included as a non-related plant. The elemental analyses of the plants were done by Wavelength Dispersive X-Ray Fluorescence (WDXRF) spectroscopy. Standard-less quantitative WDXRF analysis was carried out based on the fundamental parameter approaches. According to the standard-less analysis algorithms, there is an essential need for an accurate determination of the amount of organic material in the sample. A new approach, based on the differential thermal analysis, was successfully used for the organic material determination. The obtained results based on this approach were in a good agreement with the commonly used methods. Depending on the developed method, quantitative analysis results of eighteen elements including; Al, Br, Ca, Cl, Cu, Fe, K, Na, Ni, Mg, Mn, P, Rb, S, Si, Sr, Ti and Zn were obtained for each plant. The results of the certified reference materials of green tea (NCSZC73014, China National Analysis Center for Iron and Steel, Beijing, China) confirmed the validity of the proposed method.

  19. Intelligent Simultaneous Quantitative Online Analysis of Environmental Trace Heavy Metals with Total-Reflection X-Ray Fluorescence

    Directory of Open Access Journals (Sweden)

    Junjie Ma

    2015-05-01

    Full Text Available Total-reflection X-ray fluorescence (TXRF has achieved remarkable success with the advantages of simultaneous multi-element analysis capability, decreased background noise, no matrix effects, wide dynamic range, ease of operation, and potential of trace analysis. Simultaneous quantitative online analysis of trace heavy metals is urgently required by dynamic environmental monitoring and management, and TXRF has potential in this application domain. However, it calls for an online analysis scheme based on TXRF as well as a robust and rapid quantification method, which have not been well explored yet. Besides, spectral overlapping and background effects may lead to loss of accuracy or even faulty results during practical quantitative TXRF analysis. This paper proposes an intelligent, multi-element quantification method according to the established online TXRF analysis platform. In the intelligent quantification method, collected characteristic curves of all existing elements and a pre-estimated background curve in the whole spectrum scope are used to approximate the measured spectrum. A novel hybrid algorithm, PSO-RBFN-SA, is designed to solve the curve-fitting problem, with offline global optimization and fast online computing. Experimental results verify that simultaneous quantification of trace heavy metals, including Cr, Mn, Fe, Co, Ni, Cu and Zn, is realized on the online TXRF analysis platform, and both high measurement precision and computational efficiency are obtained.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-06-15

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

  1. Intelligent simultaneous quantitative online analysis of environmental trace heavy metals with total-reflection X-ray fluorescence.

    Science.gov (United States)

    Ma, Junjie; Wang, Yeyao; Yang, Qi; Liu, Yubing; Shi, Ping

    2015-05-06

    Total-reflection X-ray fluorescence (TXRF) has achieved remarkable success with the advantages of simultaneous multi-element analysis capability, decreased background noise, no matrix effects, wide dynamic range, ease of operation, and potential of trace analysis. Simultaneous quantitative online analysis of trace heavy metals is urgently required by dynamic environmental monitoring and management, and TXRF has potential in this application domain. However, it calls for an online analysis scheme based on TXRF as well as a robust and rapid quantification method, which have not been well explored yet. Besides, spectral overlapping and background effects may lead to loss of accuracy or even faulty results during practical quantitative TXRF analysis. This paper proposes an intelligent, multi-element quantification method according to the established online TXRF analysis platform. In the intelligent quantification method, collected characteristic curves of all existing elements and a pre-estimated background curve in the whole spectrum scope are used to approximate the measured spectrum. A novel hybrid algorithm, PSO-RBFN-SA, is designed to solve the curve-fitting problem, with offline global optimization and fast online computing. Experimental results verify that simultaneous quantification of trace heavy metals, including Cr, Mn, Fe, Co, Ni, Cu and Zn, is realized on the online TXRF analysis platform, and both high measurement precision and computational efficiency are obtained.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-09-15

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

  3. Localization of iron in rice grain using synchrotron X-ray fluorescence microscopy and high resolution secondary ion mass spectrometry

    KAUST Repository

    Kyriacou, Bianca

    2014-03-01

    Cereal crops accumulate low levels of iron (Fe) of which only a small fraction (5-10%) is bioavailable in human diets. Extensive co-localization of Fe in outer grain tissues with phytic acid, a strong chelator of metal ions, results in the formation of insoluble complexes that cannot be digested by humans. Here we describe the use of synchrotron X-ray fluorescence microscopy (XFM) and high resolution secondary ion mass spectrometry (NanoSIMS) to map the distribution of Fe, zinc (Zn), phosphorus (P) and other elements in the aleurone and subaleurone layers of mature grain from wild-type and an Fe-enriched line of rice (Oryza sativa L.). The results obtained from both XFM and NanoSIMS indicated that most Fe was co-localized with P (indicative of phytic acid) in the aleurone layer but that a small amount of Fe, often present as "hotspots", extended further into the subaleurone and outer endosperm in a pattern that was not co-localized with P. We hypothesize that Fe in subaleurone and outer endosperm layers of rice grain could be bound to low molecular weight chelators such as nicotianamine and/or deoxymugineic acid. © 2014.

  4. The analysis of thallium in geological materials by radiochemical neutron activation and x-ray fluorescence spectrometry: a comparison

    Energy Technology Data Exchange (ETDEWEB)

    McGoldrick, P.J.; Robinson, P. [Tasmania Univ., Sandy Bay, TAS (Australia)

    1993-12-31

    Carrier-based radiochemical neutron activation (RNAA) is a precise and accurate technique for the analysis of Tl in geological materials. For about a decade, until the mid-80s, a procedure modified from Keays et al. (1974) was used at the University of Melbourne to analyse for Tl in a wide variety of geological materials. Samples of powdered rock weighing several hundred milligrams each were irradiated in HIFAR for between 12 hours and 1 week, and subsequently fused with a sodium hydroxide - sodium peroxide mixture and several milligrams of inactive Tl carrier. Following acid digestion of the fusion mixture anion exchange resin was used to separate Tl from the major radioactive rock constituents. The Tl was then stripped from the resin and purified as thallium iodide and a yield measured gravimetrically. Activity from {sup 204}Tl (a {beta}-emitter with a 3 8 year half-life) was measured and Tl determined by reference to pure chemical standards irradiated and processed along with the unkowns. Detection limits for the longer irradiations were about one part per billion. Precision was monitored by repeat analyses of `internal standard` rocks and was estimated to be about five to ten percent (one standard deviation). On the other hand, X-ray fluorescence spectrometry (XRF) was seen as an excellent cost-effective alternative for thallium analysis in geological samples, down to 1 ppm. 6 refs. 1 tab., 1 fig.

  5. Interrogation of EGFR Targeted Uptake of TiO2 Nanoconjugates by X-ray Fluorescence Microscopy

    Science.gov (United States)

    Yuan, Ye; Paunesku, Tatjana; Arora, Hans; Ward, Jesse; Vogt, Stefan; Woloschak, Gayle

    2013-01-01

    We are developing TiO2 nanoconjugates that can be used as therapeutic and diagnostic agents. Nanoscale TiO2 can be surface conjugated with various molecules and has the unique ability to induce the production of reactive oxygen species after radiation activation. One way to improve the potential clinical usefulness of TiO2 nanoparticles is to control their delivery to malignant cells by targeting them to cancer cell specific antigens. Epidermal Growth Factor Receptor is one potential target that is enriched in epithelial cancers and is rapidly internalized after ligand binding. Hence, we have synthesized TiO2 nanoparticles and functionalized them with a short EGFR binding peptide to create EGFR-targeted NCs. X-ray Fluorescence Microscopy was used to image nanoconjugates within EGFR positive HeLa cells. Further labeling of fixed cells with antibodies against EGFR and Protein A nanogold showed that TiO2 nanoconjugates can colocalize with receptors at the cell’s plasma membrane. Interestingly, with increased incubation times, EGFR targeted nanoconjugates could also be found colocalized with EGFR within the cell nucleus. This suggests that EGFR-targeted nanoconjugates can bind the receptor at the cell membrane, which leads to the internalization of NC-receptor complexes and the subsequent transport of nanoconjugates into the nucleus. PMID:25284907

  6. Elemental changes in the hippocampal formation following two different formulas of ketogenic diet: an X-ray fluorescence microscopy study.

    Science.gov (United States)

    Chwiej, J; Patulska, A; Skoczen, A; Janeczko, K; Ciarach, M; Simon, R; Setkowicz, Z

    2015-12-01

    The main purpose of the following study was the determination of elemental changes occurring within hippocampal formation as a result of high-fat and carbohydrate-restricted ketogenic diet (KD). To realize it, X-ray fluorescence microscopy was applied for topographic and quantitative analysis of P, S, K, Ca, Fe, Cu, Zn and Se in hippocampal formations taken from rats fed with two different KDs and naive controls. The detailed comparisons were done for sectors 1 and 3 of the Ammon's, the dentate gyrus and hilus of dentate gyrus. The results of elemental analysis showed that the KDs induced statistically significant changes in the accumulation of P, K, Ca, Zn and Se in particular areas of hippocampal formation and these alterations strongly depended on the composition of the diets. Much greater influence on the hippocampal areal densities of examined elements was found for the KD which was characterized by a lower content of carbohydrates, higher content of fats and increased proportion of unsaturated fatty acids. The levels of P, K and Zn decreased whilst those of Ca and Se increased as a result of the treatment with the KDs.

  7. Development of microwave-assisted drying methods for sample preparation for dried spot micro-X-ray fluorescence analysis.

    Science.gov (United States)

    Link, Dirk D; Kingston, H M; Havrilla, George J; Colletti, Lisa P

    2002-03-01

    Although dried spot micro X-ray fluorescence (MXRF) is an effective analytical technique for trace elemental analysis, the sample preparation procedures currently used suffer from a number of drawbacks. These drawbacks include relatively long preparation times, lack of control of the sample preparation environment, and possibility of loss of volatile analytes during the drying process. Microwave-assisted drying offers several advantages for dried spot preparation, including control of the environment and minimized volatility because of the differences between microwave heating and conventional heating. A microwave-assisted drying technique has been evaluated for use in preparing dried spots for trace analysis. Two apparatus designs for microwave drying were constructed and tested using multielement standard solutions, a standard reference material, and a "real-world" semiconductor cleaning solution. Following microwave-assisted drying of these aqueous samples, the residues were redissolved and analyzed by ICPMS. Effective recovery was obtained using the microwave drying methods, demonstrating that the microwave drying apparatus and methods described here may be more efficient alternatives for dried spot sample preparation.

  8. X-ray Fluorescence analytical criteria to assess the fineness of ancient silver coins: Application on Ptolemaic coinage

    Energy Technology Data Exchange (ETDEWEB)

    Kantarelou, Vasiliki, E-mail: kantarelou@inp.demokritos.gr [Institute of Nuclear Physics, NCSR ' Demokritos' , Aghia Paraskevi Attikis, 153 10 (Greece); Ager, Francisco Jose, E-mail: fjager@us.es [Departamento de Fisica Aplicada I, Universidad de Sevilla, Sevilla (Spain); Centro Nacional de Aceleradores, Avda. Thomas A. Edison, 7. E-41092 Sevilla (Spain); Eugenidou, Despoina [Numismatic Museum, Athens (NMA), Athens (Greece); Chaves, Francisca [Departamento de Prehistoria y Arqueologia, Universidad de Sevilla, Sevilla (Spain); Andreou, Alexandros; Kontou, Elena; Katsikosta, Niki [Numismatic Museum, Athens (NMA), Athens (Greece); Respaldiza, Miguel Angel [Departamento de Fisica Aplicada I, Universidad de Sevilla, Sevilla (Spain); Serafin, Patrizia [Dipartimento di Beni Culturali, Musica e Spettacolo, Universita degli Studi di Roma ' Tor Vergata' , Roma (Italy); Sokaras, Dimosthenis [Institute of Nuclear Physics, NCSR ' Demokritos' , Aghia Paraskevi Attikis, 153 10 (Greece); Zarkadas, Charalambos [PANalytical B.V., 7600 AA Almelo (N