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Sample records for radioisotope x-ray fluorescence

  1. Trace elements analysis in biological samples by radioisotopic x-ray fluorescence.

    PubMed

    Cesareo, R

    1976-01-01

    The X-ray fluorescence technique, induced by radioisotopic sources, provides a very simple method for the simultaneous analysis of trace elements in biological samples. For blood, serum, platelets, etc., samples of about 0.1 ml were deposited on filter paper disks, dried, and analyzed. In such a way the "thin specimen" approximation is realized, resulting in the following advantages: The X-ray intensity of a given element is a liner function of mass per unit area over several orders of magnitude. Interelement effects became negligible. The ratio of fluorescent X-rays to scattered radiation is increased. The sensitivity of the technique for elements with atomic number ranging from about 20-92 varies from some units to some tens of parts per million by weight in 100 s measuring time, by using a gas proportional counter, and from about some tenths to some parts per million by using an X-ray semiconductor detector, in a measuring time of 10(3)-10(4)s. In such a way and with the described features, the Cl, K, Ca, Fe, Cu, Zn, Br content of several speciments of blood and serum was determined. Measurements were further carried out in order to labelling blood components with stable tracers and to detect their concentration by means of the X-ray fluorescence technique. The life span of platelets was, for example, measured after labelling platelets with stable Selenocystine. The sensitivity of the XRF technique can further be enhanced by about three orders of magnitude by using a pre-enrichment step with ion-exchange resins and liquid volumes not lower than 500 ml. Urine analyses have been carried in such a way, and copper in about 20 ml serum after selective extraction. PMID:1017430

  2. Trace element profiles in murine Lewis lung carcinoma by radioisotope-induced X-ray fluorescence.

    PubMed Central

    Frank, A. S.; Schauble, M. K.; Preiss, I. L.

    1986-01-01

    Trace element profiles of various body tissues and tumor were established during growth of the Lewis lung tumor (LLT) with the use of radioisotope-induced X-ray fluorescence (RIXRF) analysis. The LLT, a highly malignant experimental murine tumor, resembles its human counterpart, has a well-defined life cycle, and kills its host in 30 days. When compared with normal controls, Zn, Br, and Rb levels in lung, liver, and skeletal muscle and Zn and Sr levels in bone from tumor-bearing mice exhibited large fluctuations at critical points in the tumor life cycle. In addition, the 24-day primary tumor trace element profile resembled that of its tissue of origin, normal lung, and was quite different from other normal tissues studied. These findings indicate that trace element profiles may help in the diagnosis, staging, and monitoring of disease. RIXRF is an excellent technique for this purpose because it is sensitive and relatively nondestructive of samples and has multielement capabilities. Images Figure 1 p423-a PMID:3953767

  3. Student X-Ray Fluorescence Experiments

    ERIC Educational Resources Information Center

    Fetzer, Homer D.; And Others

    1975-01-01

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

  4. X-ray fluorescence holography.

    PubMed

    Hayashi, Kouichi; Happo, Naohisa; Hosokawa, Shinya; Hu, Wen; Matsushita, Tomohiro

    2012-03-01

    X-ray fluorescence holography (XFH) is a method of atomic resolution holography which utilizes fluorescing atoms as a wave source or a monitor of the interference field within a crystal sample. It provides three-dimensional atomic images around a specified element and has a range of up to a few nm in real space. Because of this feature, XFH is expected to be used for medium-range local structural analysis, which cannot be performed by x-ray diffraction or x-ray absorption fine structure analysis. In this article, we explain the theory of XFH including solutions to the twin-image problem, an advanced measuring system, and data processing for the reconstruction of atomic images. Then, we briefly introduce our recent applications of this technique to the analysis of local lattice distortions in mixed crystals and nanometer-size clusters appearing in the low-temperature phase of a shape-memory alloy. PMID:22318258

  5. Apollo 15 X-ray fluorescence experiment

    NASA Technical Reports Server (NTRS)

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

    1971-01-01

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

  6. The Mapping X-Ray Fluorescence Spectrometer (MAPX)

    NASA Technical Reports Server (NTRS)

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

    2016-01-01

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

  7. Filtered fluorescer x-ray detector

    SciTech Connect

    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.

  8. Surface-Enhanced X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Anderson, Mark

    2010-01-01

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

  9. [Radioisotope decontamination of X-ray detector (photostimulable phosphor plate)].

    PubMed

    Onuma, Yoji; Hayashi, Michiko; Hayashi, Hiroaki; Nishihara, Sadamitsu

    2012-01-01

    We tried to remove contamination of radioisotope (RI) for an X-ray detector (photostimulable phosphor plate; IP) and verified that our procedure suggested by Nishihara et al. was effective for decontamination. The procedure was as follows. First, the IP was kept for approximately twelve hours, and then it was processed [image (A)] as well as a clinical processing mode. Second, using a wet-type chemical wiper, we scavenged the IP to remove the adhered RI on its surface. Then, once again, the IP was kept for approximately fifteen hours and processed [image (B)] in order to check an effect of decontamination. Finally, the two images of (A) and (B) were analyzed using ImageJ, which can be downloaded as a free software, and a percentage of removal was calculated. The procedure was applied to two IPs using the FCR 5501 plus. In the present case, the percentage of removal was approximately 96%. The removed radioisotopes in the chemical wipers were analyzed by Ge detector. Then, (134)Cs and (137)Cs were found with activities of 2.9 4.3 Bq and 3.5 5.2 Bq, respectively. For three months after that, we cannot see black spots on the IPs owing to the contamination of the RI and there are no defects caused by decontamination using a wet-type chemical wiper. PMID:22449904

  10. Determination of Barium and selected rare-earth elements in geological materials employing a HpGe detector by radioisotope excited x-ray fluorescence

    SciTech Connect

    LaBrecque, J.J.; Preiss, I.L.

    1984-01-01

    The laterite material (geological) from Cerro Impacto was first studied by air radiometric techniques in the 1970's and was found to have an abnormally high radioactive background. Further studies showed this deposit to be rich in thorium, columbium, barium and rare-earth elements (mostly La, Ce, Pr and Nd). A similar work has been reported for the analysis of Brazil's lateritic material from Morro do Ferro to determine elemental compositions (including barium and rare-earth elements) and its relationship to the mobilization of thorium from the deposit using a Co-57 radioisotope source. The objective of this work was to develop an analytical method to determine barium and rare-earth element present in Venezuelan lateritic material from Cerro Impacto. We have employed a method before, employing a Si(Li) detector, but due to the low detection efficiencies in the rare-earth K-lines region (about 30 KeV - 40 KeV), we have decided to study the improvement in sensitivities and detection limits using an hyperpure germanium detector.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2009-09-01

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

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

    SciTech Connect

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

    2013-06-01

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

  14. PARTICULATE MATTER ELEMENTAL COMPOSITION BY X-RAY FLUORESCENCE ANALYSIS

    EPA Science Inventory

    This task is primarily concerned with the elemental characterization, by X-ray fluorescence analysis, of particulate matter (PM) collected during active or passive sampling of ambient air. The NERL X-ray fluorescence laboratory is an in-house research facility dedicated to quant...

  15. X-ray fluorescence in investigations of archaeological finds

    NASA Astrophysics Data System (ADS)

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

    2007-10-01

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

  16. Coded aperture imaging for fluorescent x-rays

    SciTech Connect

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

    2014-06-15

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

  17. Recoil splitting of x-ray-induced optical fluorescence

    SciTech Connect

    Gavrilyuk, S.; Aagren, H.; Gel'mukhanov, F.; Sun, Y.-P.; Levin, S.

    2010-03-15

    We show that the anisotropy of the recoil velocity distribution of x-ray-ionized atoms or molecules leads to observable splittings in subsequent optical fluorescence or absorption when the polarization vector of the x rays is parallel to the momentum of the fluorescent photons. The order of the magnitude of the recoil-induced splitting is about 10 {mu}eV, which can be observed using Fourier or laser-absorption spectroscopic techniques.

  18. X-ray fluorescence imaging with synchrotron radiation

    SciTech Connect

    Rivers, M.L.

    1987-01-01

    The micro-distribution of trace elements is of great interest in fields such as geochemistry, biology and material science. The synchrotron x-ray fluorescence microprobe provides a technique to quantitatively measure trace element compositions at individual points and to construct semiquantitative two dimensional maps of trace element compositions. This paper describes an x-ray fluorescence system used at the National Synchrotron Light Source.

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

    PubMed

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

    2016-02-01

    Pyroelectric X-ray generator is implemented, and an X-ray fluorescence spectrometer is accomplished by combining the pyroelectric X-ray generator with a high energy resolution silicon drift detector. Firstly, the parameters of the X-ray generator are decided by analyzing and calculating the influence of the thickness of the pyroelectriccrystal and the thickness of the target on emitted X-ray. Secondly, the emitted X-ray is measured. The energy of emitted X-ray is from 1 to 27 keV, containing the characteristic X-ray of Cu and Ta, and the max counting rate is more than 3 000 per second. The measurement also proves that the detector of the spectrometer has a high energy resolution which the FWMH is 210 eV at 8. 05 keV. Lastly, samples of Fe, Ti, Cr and high-Ti basalt are analyzed using the spectrometer, and the results are agreed with the elements of the samples. It shows that the spectrometer consisting of a pyroelectric X-ray generator and a silicon drift detector is effective for element analysis. Additionally, because each part of the spectrometer has a small volume, it can be easily modified to a portable one which is suitable for non-destructive, on-site and quick element analysis. PMID:27209767

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

    PubMed

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

    2010-10-01

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

  1. Capillary optics for micro x-ray fluorescence analysis

    SciTech Connect

    Bjeoumikhov, A.; Langhoff, N.; Bjeoumikhova, S.; Wedell, R.

    2005-06-15

    Practically achieved parameters of capillary optics are presented. A micro x-ray fluorescence (XRF) arrangement was realized by using a microfocus x-ray tube and a capillary optic. Several examples for application of micro XRF are given. It was shown that polycapillary lenses free of the 'halo effect' well suited for micro XRF of heavy elements can be manufactured. Limits of opportunities for micro XRF applications and further development for micro XRF by using capillary optics are analyzed.

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

    NASA Technical Reports Server (NTRS)

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

    1973-01-01

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

  3. Wavelength dispersive analysis with the synchrotron x ray fluorescence microprobe

    NASA Technical Reports Server (NTRS)

    Rivers, M. L.; Thorn, K. S.; Sutton, S. R.; Jones, K. W.; Bajt, S.

    1993-01-01

    A wavelength dispersive spectrometer (WDS) was tested on the synchrotron x ray fluorescence microprobe at Brookhaven National Laboratory. Compared to WDS spectra using an electron microprobe, the synchrotron WDS spectra have much better sensitivity and, due to the absence of bremsstrahlung radiation, lower backgrounds. The WDS spectrometer was successfully used to resolve REE L fluorescence spectra from standard glasses and transition metal K fluorescence spectra from kamacite.

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

    SciTech Connect

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

    1980-02-15

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

  5. Detection of terrestrial radionuclides with X-ray fluorescence analysis.

    PubMed

    Trojek, T; Čechák, T

    2015-06-01

    This paper provides an overview of analytical methods frequently used to identify terrestrial radionuclides in samples. While radioactivity is normally measured through the ionising radiation produced during the spontaneous decay of unstable atoms, selected radionuclides or their chemical elements can be quantified with instrumental techniques based on stimulated emission or counting of atoms. The advantages and disadvantages of these analytical methods are discussed. Particular attention is paid to X-ray fluorescence analysis of materials containing uranium and thorium. It is also possible to determine the area distributions of these chemical elements in samples with the use of scanning X-ray fluorescence systems. PMID:25977354

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

    NASA Technical Reports Server (NTRS)

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

    1999-01-01

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

  7. X-ray emission from the outer planets: Albedo for scattering and fluorescence of solar X rays

    NASA Astrophysics Data System (ADS)

    Cravens, T. E.; Clark, J.; Bhardwaj, A.; Elsner, R.; Waite, J. H.; Maurellis, A. N.; Gladstone, G. R.; Branduardi-Raymont, G.

    2006-07-01

    Soft X-ray emission has been observed from the low-latitude "disk" of both Jupiter and Saturn as well as from the auroral regions of these planets. The disk emission as observed by ROSAT, the Chandra X-Ray Observatory, and XMM-Newton appears to be uniformly distributed across the disk and to be correlated with solar activity. These characteristics suggest that the disk X rays are produced by (1) the elastic scattering of solar X rays by atmospheric neutrals and (2) the absorption of solar X rays in the carbon K-shell followed by fluorescent emission. The carbon atoms are found in methane molecules located below the homopause. In this paper we present the results of calculations of the scattering albedo for soft X rays. We also show the calculated X-ray intensity for a range of atmospheric abundances for Jupiter and Saturn and for a number of solar irradiance spectra. The model calculations are compared with recent X-ray observations of Jupiter and Saturn. We conclude that the emission of soft X rays from the disks of Jupiter and Saturn can be largely explained by the scattering and fluorescence of solar soft X rays. We suggest that measured X-ray intensities from the disk regions of Jupiter and Saturn can be used to constrain both the absolute intensity and the spectrum of solar X rays.

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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

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

    SciTech Connect

    Hagan, R.C.

    1982-09-01

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

  10. Archaeometrical studies using X-ray fluorescence methods

    SciTech Connect

    Pauna, Catalina; Constantinescu, B.; Constantin, F.; Bugoi, R.; Stan, D.; Vasilescu, A.

    2010-04-26

    Elemental analysis contributes to authentication (knowing the elemental composition and considering the information about the usual composition of the objects in different historical periods it can be established if the item is original or fake), provenance studies (minor and trace elements indicates ores origin and 'consequently' mines location), (relative) dating of archaeological objects (e.g. for painted items--the chemical recipes for pigments can offer information about the age of objects). The paper gives a general layout for the NIPNE Archaeometry Laboratory's applications using X-Ray Fluorescence (XRF), micro--Proton Induced X-Ray Emission (micro-PIXE), micro-Synchrotron Radiation Induced X-Ray Fluorescence (micro--SR-XRF) methods.

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

    NASA Technical Reports Server (NTRS)

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

    2013-01-01

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

  12. HIgh Rate X-ray Fluorescence Detector

    SciTech Connect

    Grudberg, Peter Matthew

    2013-04-30

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

  13. Basic studies on x-ray fluorescence analysis for active x-ray spectrometer on SELENE-2

    NASA Astrophysics Data System (ADS)

    Kusano, Hiroki; Hasebe, Nobuyuki; Nagaoka, Hiroshi; Kodama, Takuro; Oyama, Yuki; Tanaka, Reiko; Amano, Yoshiharu; Kim, Kyeong J.; Matias Lopes, Josè A.

    2013-09-01

    An active X-ray spectrometer (AXS) is now being developed as a payload candidate for the rover on SELENE-2, the next Japanese lunar exploration mission. The AXS will determine the chemical compositions of lunar rocks and regolith around the landing site. The surface of lunar rock samples will be ground using a rock abrasion tool. Thus, fundamental studies on the X-ray fluorescence analysis for lunar rocks and regolith are required to design and develop the AXS. In this study, we have investigated the X-ray fluorescence analysis in order to evaluate the effects of surface roughness of samples and the angle of incident and emergent X-rays. It was found that the fluorescent X-ray yield for low energy X-rays, i.e. the light elements, decreases at rough surface samples. This effect of surface roughness becomes small for smooth surface samples. It was also found that the fluorescent X-ray yield depends on the incident angle, which is attributed to the fact that the X-ray fluorescence occurs closer to the sample surface at larger incident angles. Since the emergent X-rays are affected by the detection geometry and surface roughness, the incident angle effect also depends on the above conditions.

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

    NASA Technical Reports Server (NTRS)

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

    2010-01-01

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

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

    PubMed

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

    2008-11-15

    As part of a comprehensive study of X-ray emission from planetary surfaces and in particular the planet Mercury, we have measured fluorescent radiation from a number of planetary analog rock samples using monochromatized synchrotron radiation provided by the BESSY II electron storage ring. The experiments were carried out using a purpose built X-ray fluorescence (XRF) spectrometer chamber developed by the Physikalisch-Technische Bundesanstalt, Germany's national metrology institute. The XRF instrumentation is absolutely calibrated and allows for reference-free quantitation of rock sample composition, taking into account secondary photon- and electron-induced enhancement effects. The fluorescence data, in turn, have been used to validate a planetary fluorescence simulation tool based on the GEANT4 transport code. This simulation can be used as a mission analysis tool to predict the time-dependent orbital XRF spectral distributions from planetary surfaces throughout the mapping phase. PMID:18855420

  16. X-ray fluorescence microscopy of olfactory receptor neurons

    NASA Astrophysics Data System (ADS)

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

    2009-09-01

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

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

    PubMed

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

    2013-01-01

    The investigation on the differences occurring in the manufacture of silver coins allows to get information on their elemental composition and represents a powerful support to the methodology to identify the producing technologies, workshops being also instrumental to distinguish between original and counterfeit ones. Aim of the present work is to study recent and old silver coins through non-destructive X-Ray Fluorescence (XRF) analysis. The XRF was applied to extend the analysis to the deepest layers of the coins; for surface layers an X-ray tube or an electron beam were employed to induce the atom fluorescence to obtain information on the surface elemental composition. Moreover, a detailed study has been performed to evaluate the influence of the surface curvature on the measurement, by deducing a proper corrective factor to keep into account in the data analysis. The elemental atomic composition was measured for each coin, mainly by means of the X-ray tube excitation for the bulk and the electron Scanning Electron Microscope (SEM) microbeam probe for the surface patina analysis. Ionization was induced by an X-ray tube using an Ag anode for the bulk and by an electron microprobe for the surface composition. X-ray detection was performed by using a semiconductor Si device cooled by a Peltier system. The Ag L-lines X-ray yield is affected by coin surface morphology and geometry. The comparison between coin spectra and standard samples, shows that the Ag quantitative analysis is influenced by error of the atomic concentration lower that 10%. PMID:24004868

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

    NASA Astrophysics Data System (ADS)

    Mendoza Cuevas, Ariadna; Perez Gravie, Homero

    2011-03-01

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

  20. X-ray fluorescence microprobe imaging in biology and medicine.

    PubMed

    Paunesku, Tatjana; Vogt, Stefan; Maser, Jörg; Lai, Barry; Woloschak, Gayle

    2006-12-15

    Characteristic X-ray fluorescence is a technique that can be used to establish elemental concentrations for a large number of different chemical elements simultaneously in different locations in cell and tissue samples. Exposing the samples to an X-ray beam is the basis of X-ray fluorescence microscopy (XFM). This technique provides the excellent trace element sensitivity; and, due to the large penetration depth of hard X-rays, an opportunity to image whole cells and quantify elements on a per cell basis. Moreover, because specimens prepared for XFM do not require sectioning, they can be investigated close to their natural, hydrated state with cryogenic approaches. Until several years ago, XFM was not widely available to bio-medical communities, and rarely offered resolution better then several microns. This has changed drastically with the development of third-generation synchrotrons. Recent examples of elemental imaging of cells and tissues show the maturation of XFM imaging technique into an elegant and informative way to gain insight into cellular processes. Future developments of XFM-building of new XFM facilities with higher resolution, higher sensitivity or higher throughput will further advance studies of native elemental makeup of cells and provide the biological community including the budding area of bionanotechnology with a tool perfectly suited to monitor the distribution of metals including nanovectors and measure the results of interactions between the nanovectors and living cells and tissues. PMID:17006954

  1. X-ray fluorescence analysis of spent reactor fuel solutions

    SciTech Connect

    Berdikov, V.V.; Iokhin, B.S.

    1987-01-01

    The present work examines the possibility of laboratory analytic control by means of a crystal-free x-ray fluorescence analysis (XRFA) installation specifically designed for this purpose with a prior selection of fluorescent emissions by energy. Monitoring by fluorescent emissions from selenium positioned in the installation along with a metering cuvette allows the exclusion of errors associated with the instability of the x-ray tube beam and the effects of the superpositioning of impulses and of dead time. Tests were made on the possibility of using hard standards, consisting of pellets of uranium-aluminum alloy in a fluoroplastic casing. Some characteristics are shown of the crystal-free x-ray fluorescent method of determining uranium concentration in the technological products from reprocessing spent fuel from a water-moderated, water-cooled reactor. The determination of the uranium content in diluted incoming solutions in the reprocessing of spent fuel from such a reactor was also tested by comparison with the results of the method of isotopic dilution concluded using mass-spectrometry.

  2. Proton-induced x-ray fluorescence CT imaging

    SciTech Connect

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

    2015-02-15

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

  3. Proton-induced x-ray fluorescence CT imaging

    PubMed Central

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

    2015-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2004-08-01

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

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

    USGS Publications Warehouse

    Groover, Krishangi; Izbicki, John

    2016-01-01

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

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

    PubMed

    Palmer, B M; McInerney, J J

    1990-05-01

    Validation studies were performed to demonstrate the effectiveness of an x-ray induced fluorescence system in quantitating regional myocardial perfusion in vivo. In a series of 13 open-chested canines, x-ray induced fluorescence was used to simultaneously monitor iodine concentration transients which arose in the left ventricular lumen and in the myocardium after the intravenous injection of an iodinated flow tracer. Deconvolution of the recorded transients produced a transfer function from which the mean transit time for the tracer to travel between the left ventricular lumen and the myocardium was calculated. Measurements of regional myocardial perfusion (Q) made by radioactive microspheres were compared with the reciprocals of the mean transit times (MTT-1) and gave a linear correlation (n = 38): MTT-1 = 0.033 + 0.069 Q, r = 0.71. Comparison of the percent change in perfusion (dQ) relative to a control study for each dog with the percent change in the respective reciprocals of the mean transit times (dMTT-1) produced a linear correlation coefficient of r = 0.88 for the regression line dMTT-1 = 0.46 dQ - 10.7. The x-ray induced fluorescence system may provide a minimally invasive means for monitoring iodine concentration transients and determining relative, if not absolute, measures of regional myocardial perfusion. PMID:2345078

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

    PubMed Central

    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

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

    PubMed

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

    2012-01-01

    Procedures for preparation of Lauha Bhasma are described in ancient texts of Ayurveda. These procedures also begin with different source material for iron such as Teekshna Lauha and Kanta Lauha etc. In the present study, we have selected different source materials viz. magnetite iron ore for Kanta Lauha and pure (Armco grade) iron turnings for Teekshna Lauha. The standard procedures of preparation of Lauha Bhasma are carried out in identical conditions for these two raw materials. The final product from the Puta are characterized by using X-ray diffraction and X-ray fluorescence spectroscopy to understanding the crystallographic form or forms of iron oxides and their composition at the end of each Puta. The iron content at the end of repeated Putas (18 for Kanta Lauha and 20 for Teekshna Lauha) have shown a decrease in case of Teekshna Lauha since the starting material is pure iron while it showed only marginal decreases in the case of Kanta Lauha because the Fe(3)O(4) of magnetite is undergoing oxidation to Fe(2)O(3). The trace elements remain within the Bhasma in the form of various oxides of Si, Al, Ca, etc. PMID:23049200

  9. Tentative study on x-ray enhancement by fluorescent emission of radiation by plasma x-ray source

    NASA Astrophysics Data System (ADS)

    Sato, Eiichi; Sagae, Michiaki; Ichimaru, Toshio; Hayasi, Yasuomi; Ojima, Hidenori; Takayama, Kazuyoshi; Ido, Hideaki; Sakamaki, Kimio; Tamakawa, Yoshiharu

    1999-09-01

    Tentative study on characteristic x-ray enhancement by fluorescent emission of radiation by plasma x-ray source is described. The enhancement was performed by the plasma flash x-ray generator having a cold-cathode triode. And the generator employs a high-voltage power supply, a low-impedance coaxial transmission line with a gap switch, a high-voltage condenser with a capacity of 200 nF, a turbo-molecular pump, a thyristor pulser as a trigger device, and a flash x-ray tube. The high-voltage main condenser is charged up to 60 kV by the power supply, and the electric charges in the condenser are discharged to the tube after triggering the cathode electrode. The flash x-rays are then produced. The x-ray tube is of a demountable triode that is connected to the turbo molecular pump with a pressure of approximately 1 mPa. As the electron flows from the cathode electrode are roughly converged to the target by the electric field in the tube, the plasma x-ray source, which consists of metal ions and electrons, forms by the target evaporating. Both the tube voltage and current displayed damped oscillations, and their peak values increased according to increases in the charging voltage. In the present work, the peak tube voltage was almost equivalent to the initial charging voltage of the main condenser, and the peak current was less than 30 kA. The characteristic x-ray intensity substantially increased according to the growth in the plasma x-ray source. When the linear plasma x-ray source formed, the bremsstrahlung x-rays were absorbed without using a monochromatic filter, and high- intensity characteristic x-rays were produced.

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

    SciTech Connect

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

    1986-01-01

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

  11. Micro-X-ray Fluorescence in Food Forensics

    NASA Astrophysics Data System (ADS)

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

    2011-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-07-01

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

  13. The Apollo 15 X-ray fluorescence experiment

    NASA Technical Reports Server (NTRS)

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

    1972-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Visco, A.

    2003-12-01

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

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

    PubMed

    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

    2016-09-01

    Owing to its extreme sensitivity, quantitative mapping of elemental distributions via X-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. PMID:27577770

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

    NASA Astrophysics Data System (ADS)

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

    2005-12-01

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

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

    NASA Technical Reports Server (NTRS)

    Eldridge, Hudson B.

    1988-01-01

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

  18. X-ray fluorescence analysis of titanium alloys.

    PubMed

    Vassilaros, G L; McKaveney, J P

    1969-02-01

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

  19. Feasibility of x ray fluorescence for spent fuel safeguards

    SciTech Connect

    Freeman, Corey Ross; Mozin, Vladimir; Tobin, Stephen J; Fensin, Michael L; White, Julia M; Croft, Stephen; Stafford, Alissa; Charlton, William

    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

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

    NASA Astrophysics Data System (ADS)

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

    1999-09-01

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

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

    PubMed

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

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

  2. Using X-ray Fluorescence to Date Petroglyphs

    NASA Astrophysics Data System (ADS)

    McNeil, James

    2009-10-01

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

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

    PubMed Central

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

    2013-01-01

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

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

    NASA Technical Reports Server (NTRS)

    Hertel, R.; Holm, M.

    1973-01-01

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

  5. Determination of thorium by fluorescent x-ray spectrometry

    USGS Publications Warehouse

    Adler, I.; Axelrod, J.M.

    1955-01-01

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

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

    SciTech Connect

    Das, Gangadhar Tiwari, M. K.; Singh, A. K.; Ghosh, Haranath

    2015-06-24

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

  7. Soil characterization by energy dispersive X-ray fluorescence: sampling strategy for in situ analysis.

    PubMed

    Custo, Graciela; Boeykens, Susana; Dawidowski, L; Fox, L; Gómez, D; Luna, F; Vázquez, Cristina

    2005-07-01

    This work describes a sampling strategy that will allow the use of portable EDXRF (energy dispersive X-ray fluorescence) instruments for "in situ" soil analysis. The methodology covers a general approach to planning field investigations for any type of environmental studies and it was applied for a soil characterization study in the zone of Campana, Argentina, by evaluating data coming from an EDXRF spectrometer with a radioisotope excitation source. Simulating non-treated sampled as "in situ" samples and a soil characterization for Campana area was intended. "In situ" EDXRF methodology is a powerful analytical modality with the advantage of providing data immediately, allowing a fast general screening of the soil composition. PMID:16038489

  8. Quo Vadis total reflection X-ray fluorescence?

    NASA Astrophysics Data System (ADS)

    Pahlke, Siegfried

    2003-12-01

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

  9. Fast X-Ray Fluorescence Microtomography of Hydrated Biological Samples

    PubMed Central

    Lombi, Enzo; de Jonge, Martin D.; Donner, Erica; Kopittke, Peter M.; Howard, Daryl L.; Kirkham, Robin; Ryan, Chris G.; Paterson, David

    2011-01-01

    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. PMID:21674049

  10. Sensitivity of in vivo X-ray fluorescence determination of skeletal lead stores

    SciTech Connect

    Sokas, R.K.; Besarab, A.; McDiarmid, M.A.; Shapiro, I.M.; Bloch, P. )

    1990-09-01

    Eighteen patients with known past occupational lead exposure underwent parenteral diagnostic chelation with ethylenediaminetetraacetic acid and x-ray fluorescent determination of in vivo skeletal lead stores at the distal styloid process of the ulna and at the temporal base bone using a cobalt 57 source and measuring lead Ka x-rays. X-ray fluorescent lead measurements in both locations correlated with results of diagnostic chelation. Using a post-chelation urinary excretion of greater than 600 micrograms lead/24 h as the definition of high-lead stores, sensitivity of x-ray fluorescence at the wrist and temple was 56% and 39%, respectively.

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

    DOEpatents

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

    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.

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

    DOEpatents

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

    2009-04-14

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

  13. X-ray fluorescence from rough rocky surfaces of asteroids

    NASA Astrophysics Data System (ADS)

    Okada, T.

    2014-07-01

    X-ray fluorescence (XRF) from orbit is a frequently-used technique to determine the elemental composition of atmosphereless planetary bodies. So far, XRF observations have been conducted for asteroids by the Near-Earth Asteroid Rendezvous Shoemaker mission at (433) Eros [1] and the Hayabusa mission at (25143) Itokawa [2]. There has been difficulties to interpret the XRF data to derive the composition quantitatively. One of the reasons is the surface-roughness effect. We have investigated the XRF intensity influenced by a powdery surface as an analogue to fine regolith [3,4]. However, the surfaces of asteroids explored by the spacecraft at, e.g., (25143) Itokawa or (433) Eros, were not always covered with fine regolith but with pebbles or boulders. Thus, we have performed laboratory experiments to study the roughness effect for rocky surfaces to interpret the XRF observations of those asteroids and the observations of future missions. For the powdery surface, we have obtained the following results: 1) the XRF with lower energy is more effective for the same roughness; 2) the XRF intensity decreases for rougher surfaces but converges to a constant value almost 50--60 % of that of a flat surface; and 3) the XRF intensity decreases for larger phase angles, but does not change so for a varying incident angle when when the phase angle remains fixed. We started the experiments for rocky surfaces to investigate the elemental composition of natural unprepared rocks as well as ground rocks for past and future planetary missions. We prepared the basaltic rock samples with different surface roughness. The roughness of the rock surface is measured with a laser microscope to obtain the three-dimensional surface features and characterize the roughness in <10, 30, 60, 100-micron scales by a rectangular function as in our previous studies. We used the X-ray generator (RIGAKU RINT-2000) using an X-ray tube of Cr-target (V-filter) at 20 kV and 10mA, and detected with the Si-PIN diode

  14. Measurement uncertainty in Total Reflection X-ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Floor, G. H.; Queralt, I.; Hidalgo, M.; Marguí, E.

    2015-09-01

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

  15. Continuous Flow Cryostat for X-Ray Fluorescence

    SciTech Connect

    Weng, T.-C.; Linden, Peter J. E. M. van der; Glatzel, Pieter; Lapras, Christophe; Krzyzowski, Michael

    2010-06-23

    A continuous Helium flow cryostat was designed and built by Cryovac GMbH to specifications given by ESRF beamline ID26. The beamline has constructed a high energy resolution X-ray emission spectrometer using multiple spherically bent analyser crystals, together with the sample and detector on a vertical Rowland circle. The double shrouded cryostat has a low profile designed to fit into the spectrometer setup, the lowest detector position allows for a Bragg angle of 85 degrees with a 1 meter diameter Rowland circle. The cryostat has a temperature range of 5 to 300 Kelvin on the sample holder which is cooled by static Helium exchange gas. The cryostat has triple windows for beam entrance, transmission and fluorescence; the latter offers an opening angle of 80 degrees horizontally and 50 degrees vertically. The cryostat can be configured to work in two different operation modes: translation or rotation. The translation mode offers a displacement of 50 mm to accommodate multiple samples on the sample holder. The rotation mode is used for polarisation studies on single crystals.We show recent results obtained on Chromium containing molecular complexes; data collection was done at a temperature of 10 Kelvin to avoid radiation damage.

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

    NASA Astrophysics Data System (ADS)

    Havrilla, George J.; Miller, Thomasin C.

    2005-06-01

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

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

    SciTech Connect

    1998-12-01

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

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

    SciTech Connect

    Havrilla, George J.; Miller, Thomasin C.

    2005-06-15

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

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

    SciTech Connect

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

    2013-06-15

    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).

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

    USGS Publications Warehouse

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

    1973-01-01

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

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

    PubMed

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

    2012-04-15

    Multimodal imaging technique is an alternative approach to improve sensitivity of early cancer diagnosis. In this study, highly fluorescent and strong X-ray absorption coefficient gold nanoclusters (Au NCs) are synthesized as dual-modality imaging contrast agents (CAs) for fluorescent and X-ray dual-modality imaging. The experimental results show that the as-prepared Au NCs are well constructed with ultrasmall sizes, reliable fluorescent emission, high computed tomography (CT) value and fine biocompatibility. In vivo imaging results indicate that the obtained Au NCs are capable of fluorescent and X-ray enhanced imaging. PMID:22289255

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

    PubMed Central

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

    2014-01-01

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

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

    PubMed

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

    2012-11-01

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

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

    PubMed

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

    2010-01-01

    This paper deals with an investigation of ceramic archaeological finds with the use of in-situ X-ray fluorescence analysis. Firstly, three configurations of X-ray fluorescence analyzers constructed and used at the Czech Technical University in Prague are described and compared for use in a non-destructive survey of siliceous materials. Detection limits, depth of analysis, the relation of the analyzed area, the homogeneity of the samples, and variations in the element concentrations are discussed. Secondly, many shards of postmediaeval pottery from Southern Moravia are analyzed with X-ray fluorescence analysis and some of them also with electron microprobe analysis. Selected results are described. PMID:19914840

  5. RADIOCHEMICAL ANALYSIS BY HIGH SENSITIVITY DUAL-OPTIC MICRO X-RAY FLUORESCENCE

    EPA Science Inventory

    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...

  6. A 30 nm-resolution hard X-ray microscope with X-ray fluorescence mapping capability at BSRF.

    PubMed

    Yuan, Qingxi; Zhang, Kai; Hong, Youli; Huang, Wanxia; Gao, Kun; Wang, Zhili; Zhu, Peiping; Gelb, Jeff; Tkachuk, Andrei; Hornberger, Benjamin; Feser, Michael; Yun, Wenbing; Wu, Ziyu

    2012-11-01

    A full-field transmission X-ray microscope (TXM) operating continuously from 5 keV to 12 keV with fluorescence mapping capability has been designed and constructed at the Beijing Synchrotron Radiation Facility, a first-generation synchrotron radiation facility operating at 2.5 GeV. Spatial resolution better than 30 nm has been demonstrated using a Siemens star pattern in both absorption mode and Zernike phase-contrast mode. A scanning-probe mode fluorescence mapping capability integrated with the TXM has been shown to provide 50 p.p.m. sensitivity for trace elements with a spatial resolution (limited by probing beam spot size) of 20 µm. The optics design, testing of spatial resolution and fluorescence sensitivity are presented here, including performance measurement results. PMID:23093765

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

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

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

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

    PubMed

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

    2014-04-01

    The high-resolution von Hamos bent crystal spectrometer of the University of Fribourg was upgraded with a focused X-ray beam source with the aim of performing micro-sized X-ray fluorescence (XRF) measurements in the laboratory. The focused X-ray beam source integrates a collimating optics mounted on a low-power micro-spot X-ray tube and a focusing polycapillary half-lens placed in front of the sample. The performances of the setup were probed in terms of spatial and energy resolution. In particular, the fluorescence intensity and energy resolution of the von Hamos spectrometer equipped with the novel micro-focused X-ray source and a standard high-power water-cooled X-ray tube were compared. The XRF analysis capability of the new setup was assessed by measuring the dopant distribution within the core of Er-doped SiO2 optical fibers. PMID:24784587

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

    SciTech Connect

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

    2014-04-15

    The high-resolution von Hamos bent crystal spectrometer of the University of Fribourg was upgraded with a focused X-ray beam source with the aim of performing micro-sized X-ray fluorescence (XRF) measurements in the laboratory. The focused X-ray beam source integrates a collimating optics mounted on a low-power micro-spot X-ray tube and a focusing polycapillary half-lens placed in front of the sample. The performances of the setup were probed in terms of spatial and energy resolution. In particular, the fluorescence intensity and energy resolution of the von Hamos spectrometer equipped with the novel micro-focused X-ray source and a standard high-power water-cooled X-ray tube were compared. The XRF analysis capability of the new setup was assessed by measuring the dopant distribution within the core of Er-doped SiO{sub 2} optical fibers.

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

    DOEpatents

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

    2010-12-28

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

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

    NASA Astrophysics Data System (ADS)

    Bergmann, Uwe; Knox, Keith T.

    2009-01-01

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

  12. Multiplexed biomarker detection using x-ray fluorescence of composition-encoded nanoparticles

    SciTech Connect

    Hossain, Mainul; Wang Chaoming; Su Ming

    2010-12-27

    Multiple DNA and protein biomarkers have been detected based on characteristic x-ray fluorescence of a panel of metal and alloy nanoparticles, which are modified with ligands of biomarkers to create a one-to-one correspondence and immobilized on ligand-modified substrates after forming complexes with target biomarkers in three-strand or sandwich configuration. By determining the presence and concentration of nanoparticles using x-ray fluorescence, the nature and amount of biomarkers can be detected with limits of 1 nM for DNA and 1 ng/ml for protein. By combining high penetrating ability of x-rays, this method allows quantitative imaging of multiple biomarkers.

  13. ISS Ammonia Leak Detection Through X-Ray Fluorescence

    NASA Technical Reports Server (NTRS)

    Camp, Jordan; Barthelmy, Scott; Skinner, Gerry

    2013-01-01

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

  14. Two facets of the x-ray microanalysis at low voltage: The secondary fluorescence x-rays emission and the microcalorimeter energy-dispersive spectrometer

    NASA Astrophysics Data System (ADS)

    Demers, Hendrix

    The best spatial resolution, for a microanalysis with a scanning electron microscope (SEND, is achieved by using a low voltage electron beam. But the x-ray microanalysis was developed for high electron beam energy (greater than 10 keV). Also, the specimen will often contain light and medium elements and the analyst will have to use a mixture of K, L, and sometime M x-ray peaks for the x-ray microanalysis. With a mixture of family lines, it will be common to have secondary fluorescence x-rays emission by K--L and L--K interactions. The accuracy of the fluorescence correction models presently used by the analyst are not well known for these interactions. This work shows that the modified secondary fluorescence x-rays emission correction models can improve the accuracy of the microanalysis for K--L and L--K interactions. The general equation derived in this work allows the identification of three factors which influence the secondary fluorescence x-rays emission. The fluorescence production factor epsilonƒ can be used to predict the importance of the secondary fluorescence x-rays emission. A large value of epsilonƒ indicates that a fluorescence correction is needed. Another disadvantage of using a low voltage is that there are more frequent occurrences of x-ray peaks overlap. A new microanalysis instruments that combines the high-spatial resolution and high-energy resolution for x-ray detection is needed. The microcalorimeter energy-dispersive spectrometer (muEDS) should improve the low voltage microanalysis, but the maturity of this technology has to be evaluated first. One of the first commercial muEDS for x-ray microanalysis in a SEM is studied and analyzed in this work. This commercial muEDS has an excellent energy resolution (˜ 15 eV) and can detect x-rays of low energy. This x-ray detector can be used as a high-spatial resolution and high-energy resolution microanalysis instrument. There are still hurdles that this technology must overcome before its

  15. Portable x-ray fluorescence spectrometer for coating thickness measurement

    SciTech Connect

    Carapelle, Alain; Fleury-Frenette, Karl; Collette, Jean-Paul; Garnir, Henri-Pierre; Harlet, Philippe

    2007-12-15

    A handheld x-ray spectrometer has been realized and tested. The purpose of the device is to measure the thickness of coated samples in the range of 1-1500 nm in an industrial environment. Accuracy of {approx}3% has been achieved in this range with a measurement time of 1 min. Automated software has been implemented to allow utilization by a nonspecialist operator. An automated calibration procedure, based on measurements of reference samples, is used.

  16. Determination of L X-ray fluorescence parameters for Ho, Lu, W, Hg and Bi.

    PubMed

    Turhan, M F; Durak, R; Akman, F

    2014-07-01

    In this work, L X-ray fluorescence cross sections, L sub-shell fluorescence yields and level widths and radiative vacancy transfer probabilities of L sub-shells to Mi, Ni and Oi sub-shells were measured for the elements Ho, Lu, W, Hg and Bi. Energy dispersive X-ray fluorescence (EDXRF) technique was used to measure L X-ray photons. To obtain related parameters, we used 59.54 keV gamma photons of (241)Am radioactive point source. Emitted L X-ray photons from targets were collected by means of a Si(Li) detector with resolution of 180 eV at 5.9 keV. The present results are generally in a good agreement with theoretical calculations and the other results obtained in the literature, within their range considering experimental uncertainty. PMID:24631748

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

    SciTech Connect

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

    2005-06-15

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

  18. Numerical simulation of X-ray fluorescence production using MCNPX code

    NASA Astrophysics Data System (ADS)

    Kim, Kyeong Ja; Park, Junghun Park

    Numerical simulation for the production of X-ray fluorescence by an active X-ray spectrometer was accomplished by MCNPX (Monte Carlo N-particle eXtended) Code. Purpose of this study is to cross check between the simulation result and the actual measurement to validate the numerical simulation for prospective usage for various possible cases of measurements which are not easily accessible in a laboratory environment. This study was initiated as a conjunction of Phase A study for the SELENE-2 science payload proposed in 2011. The active X-ray Spectrometer includes an X-ray spectrometer and a pyroelectric crystal-used X-ray generator. For Phase A study, we used both XRS and XRG available from the commercial company, Amptek Inc. Numerical simulation is important to optimize both instrument design and geometry of measurement to perform the best measurement output of an experiment planned. The main purpose of this study is to understand the production of X-ray fluorescence by an active X-ray spectrometer which could be onboard for future planetary spacecraft. For the numerical simulation, we used the lunar simulant FSJ-1 composition, and the input parameters for X-ray flux and energy distribution were accessed from the information of the X-ray generator, Cool-X. The parameters for geometry setting were defined as the experimental setting used for the actual measurement. It was found that the spectrum of numerical simulation is compared well with the actual measurement at the laboratory setting with respect to the number of elements, peak counts, and energy spectrum. To find optimal distance and geometry settings toward the production of X-ray fluorescence, multiple simulations at various geometry settings are currently under investigation.

  19. A tube-excited x-ray fluorescence spectrometer for use in small-diameter boreholes

    SciTech Connect

    Reeves, J.H.; Arthur, R.J.; Brodzinski, R.L.; Shepard, C.L.

    1995-04-01

    A portable in-situ x-ray fluorescence analytical system that uses an x-ray tube excitation source and a cooled Si(Li) spectrometer for detecting characteristic emission x rays has been developed for use in small-diameter wells and boreholes. The 15-watt, iron-anode x-ray tube operates up to 30 kV. Three wells at the Sandia National Laboratory Chemical Waste Landfill, lined with 76 {mu} thick polyethylene, were logged specifically for Cr contamination. Detection limits below 50 ppM were achieved with counting intervals of 600 seconds and with the Si(Li) detector operating at 450-eV resolution (full width at half maximum [FWHM] for the Mn K-alpha x ray).

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

    PubMed

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

    2012-02-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-12-01

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

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

    SciTech Connect

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

    2013-05-06

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

  3. X-ray fluorescence analysis for prediction of Space Shuttle solid rocket motor performance

    NASA Technical Reports Server (NTRS)

    Pulsipher, H. G.

    1978-01-01

    Analysis of uncured solid propellant by X-ray fluorescence has been conducted on mixes prepared for four development motors produced for the Space Shuttle SRM Project. X-ray readings for chlorine (ammonium perchlorate) and iron (ferric oxide) were recorded for each mix during processing of the propellant. These values were used to predict burning rates for uncured acceptance, uncured acoustic emission and cured acoustic emission strands. Predicted burning rates all fell within control limits and when compared to actual burning rates, most were within experimental error. The X-ray analysis required one-third the time of current methods and met casting schedules.

  4. Gadolinium concentration analysis in brain phantom by X-ray fluorescence.

    PubMed

    Almalki, Musaed; Majid, Samir Abdul; Butler, Philip H; Reinisch, Lou

    2010-06-01

    We have measured the X-ray fluorescence from gadolinium as a function of concentration and position in tumors of different sizes and shapes in a head phantom. The gadolinium fluorescence was excited with a 36 GBq Am-241 source. The fluorescence signal was detected with a CdTe detector and a multi-channel analyzer. The fluorescence peak was clearly separated from the scattered X-rays. Concentrations of 5.62-78.63 mg/ml of Gd ion were used in 1, 2, and 3 cm diameter spherical tumors and a 2x4 cm oblate spheroid tumor. The data show trends approaching saturation for the highest concentrations, probably due to reabsorption in the tumor. A comparison of X-ray photographic imaging and densitometer measurements to determine concentration is also presented. PMID:20596811

  5. An X-ray fluorescence spectrometer and its applications in materials studies

    NASA Technical Reports Server (NTRS)

    Singh, J. J.; Han, K. S.

    1977-01-01

    An X-ray fluorescence system based on a Co(57) gamma-ray source has been developed. The system was used to calculate the atomic percentages of iron implanted in titanium targets. Measured intensities of Fe (k-alpha + k-beta) and Ti (k-alpha + k-beta) X-rays from the Fe-Ti targets are in good agreement with the calculated values based on photoelectric cross sections of Ti and Fe for the Co(57) gamma rays.

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

    NASA Technical Reports Server (NTRS)

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

    1991-01-01

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

  7. Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

    SciTech Connect

    Liu, Ying Imashuku, Susumu; Sasaki, Nobuharu; Ze, Long; Kawai, Jun; Takano, Shotaro; Sohrin, Yoshiki; Seki, Hiroko; Miyauchi, Hiroya

    2014-05-15

    In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient to determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.

  8. X-ray fluorescence spectrometer onboard Hayabusa: instrument, science and observation plan

    NASA Astrophysics Data System (ADS)

    Okada, T.; Shirai, K.; Yamamoto, Y.; Arai, T.; Ogawa, K.; Kato, M.; Hayabusa Xrs Team

    We have developed a CCD-based X-ray fluorescence spectrometer, XRS, onboard the HAYABUSA spacecraft, with heritage technology from the X-ray fluorescence and atmospheric detector onboard the S310-28 sounding rocket experiment. Its scientific objectives are (1) to determine surface major elemental composition of asteroid 25143 Itokawa (1998SF36), (2) to map longitudinal variation of elements, if it exists, by asteroid rotation, (3) to inform on surface microscopic roughness via measurement of surface regolith's particle size effect in X-ray fluorescence, and (4) to observe X-ray bodies and X-ray cosmic backgrounds. At the earth swing-by phase, we have a plan to observe X-rays from the earth and moon. In addition, thermal design of the XRS is suitable, and examined in the spacecraft thermal vacuum test, for thermal emission study of asteroid to observe during the asteroid touchdown phase for sample collection, because the XRS has a large radiator at the asteroid pointing direction and the chassis is thermally isolated from the structure of spacecraft. We will present details of the XRS instrumentation, scientific objectives, and future observation plans, together with some results of pre-flight laboratory experiments and preliminary results of in-flight observations.

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

    NASA Technical Reports Server (NTRS)

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

    1972-01-01

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

  10. Apollo 16 geochemical X-ray fluorescence experiment - Preliminary report.

    NASA Technical Reports Server (NTRS)

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

    1972-01-01

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

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

    PubMed

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

    1972-07-21

    The lunar surface was mapped with respect to magnesium, aluminum, and silicon as aluminum/ silicon and magnesium/ silicon intensity ratios along the projected ground tracks swept out by the orbiting Apollo 16 spacecraft. The results confirm the observations made during the Apollo 15 flight and provide new data for a number of features not covered before. The data are consistent with the idea that the moon has a widespread differentiated crust (the highlands). The aluminum/ silicon and magnesium/ silicon concentration ratios correspond to those for anorthositic gabbros through gabbroic anorthosites or feldspathic basalts. The x-ray results suggest the occurrence of this premare crust or material similar to it at the Descartes landing site. PMID:17815621

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

    SciTech Connect

    Blankespoor, S.C. |

    1993-12-01

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

  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

    NASA Astrophysics Data System (ADS)

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

    2009-07-01

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

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

    USGS Publications Warehouse

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

    1990-01-01

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

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

    SciTech Connect

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

    2014-11-15

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

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

    SciTech Connect

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

    2015-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    2005-01-01

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

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

    PubMed Central

    Cong, Wenxiang; Shen, Haiou; Wang, Ge

    2011-01-01

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

  19. Three-dimensional x-ray fluorescence mapping of a gold nanoparticle-loaded phantom

    SciTech Connect

    Ren, Liqiang; Wu, Di; Li, Yuhua; Liu, Hong; Wang, Ge; Wu, Xizeng

    2014-03-15

    Purpose : X-ray fluorescence (XRF) is a promising technique with sufficient specificity and sensitivity for identifying and quantifying features in small samples containing high atomic number (Z) materials such as iodine, gadolinium, and gold. In this study, the feasibility of applying XRF to early breast cancer diagnosis and treatment is studied using a novel approach for three-dimensional (3D) x-ray fluorescence mapping (XFM) of gold nanoparticle (GNP)-loaded objects in a physical phantom at the technical level. Methods : All the theoretical analysis and experiments are conducted under the condition of using x-ray pencil beam and a compactly integrated x-ray spectrometer. The penetrability of the fluorescence x-rays from GNPs is first investigated by adopting a combination of BR12 with 70 mm/50 mm in thickness on the excitation/emission path to mimic the possible position of tumor goldin vivo. Then, a physical phantom made of BR12 is designed to translate in 3D space with three precise linear stages and subsequently the step by step XFM scanning is performed. The experimental technique named as background subtraction is applied to isolate the gold fluorescence from each spectrum obtained by the spectrometer. Afterwards, the attenuations of both the incident primary x-ray beam with energies beyond the gold K-edge energy (80.725 keV) and the isolated gold K{sub α} fluorescence x-rays (65.99 –69.80 keV) acquired after background subtraction are well calibrated, and finally the unattenuated K{sub α} fluorescence counts are used to realize mapping reconstruction and to describe the linear relationship between gold fluorescence counts and corresponding concentration of gold solutions. Results : The penetration results show that the goldK{sub α} fluorescence x-rays have sufficient penetrability for this phantom study, and the reconstructed mapping results indicate that both the spatial distribution and relative concentration of GNPs within the designed BR12 phantom

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

    SciTech Connect

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

    2007-08-08

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

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

    SciTech Connect

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

    2014-06-15

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

  3. Polychromatic excitation improves detection limits in total reflection X-ray fluorescence analysis compared with monochromatic excitation.

    PubMed

    Kunimura, Shinsuke; Kawai, Jun

    2010-08-01

    Detection limits obtained by a portable total reflection X-ray fluorescence (TXRF) spectrometer with or without a monochromator are compared. A 1 W X-ray tube (tube voltage: 20 kV) is used in this spectrometer. Polychromatic excitation improves the detection limits in TXRF analysis with the low power X-ray tube compared with monochromatic excitation. A detection limit of 26 pg is achieved for Co when using the weak polychromatic X-rays. PMID:20535410

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

    NASA Astrophysics Data System (ADS)

    Ignatyev, Konstantin; Huwig, Kathy; Harvey, Ralph; Ishii, Hope; Bradley, John; Luening, Katharina; Brennan, Sean; Pianetta, Piero

    2007-01-01

    X-ray fluorescence microCT (computed tomography) is a novel technique that allows non-destructive determination of the 3D distribution of chemical elements inside a sample. This is especially important in samples for which sectioning is undesirable either due to the risk of contamination or the requirement for further analysis by different characterization techniques. Developments made by third generation synchrotron facilities and laboratory X-ray focusing systems have made these kinds of measurements more attractive by significantly reducing scan times and beam size. First results from the x-ray fluorescence microCT experiments performed at SSRL beamline 6-2 are reported here. Beamline 6-2 is a 54 pole wiggler that uses a two mirror optical system for focusing the x-rays onto a virtual source slit which is then reimaged with a set of KB mirrors to a (2 × 4) μm2 beam spot. An energy dispersive fluorescence detector is located in plane at 90 degrees to the incident beam to reduce the scattering contribution. A PIN diode located behind the sample simultaneously measures the x-ray attenuation in the sample. Several porous micrometeorite samples were measured and the reconstructed element density distribution including self-absorption correction is presented. Ultimately, this system will be used to analyze particles from the coma of comet Wild-2 and fresh interstellar dust particles both of which were collected during the NASA Stardust mission.

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

    SciTech Connect

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

    2006-08-23

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

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

    SciTech Connect

    Ignatyev, Konstantin; Luening, Katharina; Brennan, Sean; Pianetta, Piero; Huwig, Kathy; Harvey, Ralph; Ishii, Hope; Bradley, John

    2007-01-19

    X-ray fluorescence microCT (computed tomography) is a novel technique that allows non-destructive determination of the 3D distribution of chemical elements inside a sample. This is especially important in samples for which sectioning is undesirable either due to the risk of contamination or the requirement for further analysis by different characterization techniques. Developments made by third generation synchrotron facilities and laboratory X-ray focusing systems have made these kinds of measurements more attractive by significantly reducing scan times and beam size. First results from the x-ray fluorescence microCT experiments performed at SSRL beamline 6-2 are reported here. Beamline 6-2 is a 54 pole wiggler that uses a two mirror optical system for focusing the x-rays onto a virtual source slit which is then reimaged with a set of KB mirrors to a (2 x 4) {mu}m2 beam spot. An energy dispersive fluorescence detector is located in plane at 90 degrees to the incident beam to reduce the scattering contribution. A PIN diode located behind the sample simultaneously measures the x-ray attenuation in the sample. Several porous micrometeorite samples were measured and the reconstructed element density distribution including self-absorption correction is presented. Ultimately, this system will be used to analyze particles from the coma of comet Wild-2 and fresh interstellar dust particles both of which were collected during the NASA Stardust mission.

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

    SciTech Connect

    Collins, Michael L; Havrilla, George J

    2009-01-01

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

  8. Grazing exit micro X-ray fluorescence analysis of a hazardous metal attached to a plant leaf surface using an X-ray absorber method.

    PubMed

    Awane, Tohru; Fukuoka, Shintaro; Nakamachi, Kazuo; Tsuji, Kouichi

    2009-05-01

    If human beings or animals repeatedly ingest plant leaves contaminated with minute quantities of hazardous metals (Pb, As, Hg, Cd, etc.), the metals will gradually accumulate in their bodies. When the quantities of the metals in the bodies reach toxic levels, they may cause serious symptoms of poisoning. Therefore, it is significant to detect and analyze the minute quantities of hazardous metals that attach to plant leaves in terms of epidemiology and disease prevention. We developed grazing exit micro X-ray fluorescence analysis (GE-micro-XRF), which was expected to analyze the localized surface of an aqueous plant leaf with a much faster and simpler sample treatment than with conventional analytical methods, to detect Pb attached to a surface of a leaf of Camellia hiemalis. A micro X-ray beam was produced by using a polycapillary X-ray lens. GE-v-XRF is a grazing exit X-ray analysis (GE-XA) method in which X-rays emitted from only the near-surface region of a specimen are selectively detected under a grazing exit angle condition (extremely low exit angle near 0 degrees). In any GE-XA method, X-rays emitted from inside the specimen must be absorbed inside the specimen and attenuated when X-rays pass through the specimen. However, we deduced that X-rays emitted from inside aqueous organic material such as a plant leaf are scarcely absorbed because X-ray absorption in any aqueous organic material is much smaller than that in most metallic and semiconductor materials, which was analyzed with GE-XA methods. Therefore, we have developed a novel GE-micro-XRF method in which a chip of a silicon wafer is placed between the analyzed leaf and an X-ray detector as an absorber of the X-rays emitted from inside the leaf. As a result of GE-XRF analysis of a leaf dipped in Pb standard solution using the X-ray absorber, we have for the first time selectively detected X-rays emitted from the near-surface region of an aqueous plant leaf. Therefore, we have detected X-rays emitted

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

    NASA Astrophysics Data System (ADS)

    Sitko, Rafał

    2009-11-01

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

  10. X-ray microprobe synchroton radiation X-ray fluorescence application on human teeth of renal insufficiency patients

    NASA Astrophysics Data System (ADS)

    Marques, A. F.; Marques, J. P.; Casaca, C.; Carvalho, M. L.

    2004-10-01

    This work reports on the measurements of elemental profiles in teeth collected from patients with renal insufficiency. Elemental concentrations of Ti, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Rb Sr and Pb in different parts of teeth from patients with renal insufficiency are discussed and correlated with the corresponding values for healthy citizens. Both situations, patients with and without dialysis treatment were studied. The purpose of this work is to point out the influence of renal insufficiency together with long dialysis treatment, on teeth elemental content. An X-ray fluorescence set-up with microprobe capabilities, installed at the LURE synchrotron (France) was used for elemental determination. The resolution of the synchrotron microprobe was 100 μm and the energy of the incident photons was 19 keV. Teeth of citizens with renal insufficiency and those submitted since several years to dialysis treatment show a similar concentration with teeth of healthy subjects in what concerns the elemental distribution for Mn, Fe, Cu, Zn and Sr. However, higher levels of Pb were found in pulp region of diseased citizens when compared to values of healthy people. Very low concentrations of Ti, Co, Ni, Se, Br and Rb were found in all the analysed teeth. No difference was found in patients with and without dialysis treatment.

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

    PubMed

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

    2012-02-01

    Hard X-ray fluorescence microscopy and magnified phase contrast imaging are combined to obtain quantitative maps of the projected metal concentration in whole cells. The experiments were performed on freeze dried cells at the nano-imaging station ID22NI of the European Synchrotron Radiation Facility (ESRF). X-ray fluorescence analysis gives the areal mass of most major, minor and trace elements; it is validated using a biological standard of known composition. Quantitative phase contrast imaging provides maps of the projected mass and is validated using calibration samples and through comparison with Atomic Force Microscopy and Scanning Transmission Ion Microscopy. Up to now, absolute quantification at the sub-cellular level was impossible using X-ray fluorescence microscopy but can be reached with the use of the proposed approach. PMID:22182730

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

    DOE PAGESBeta

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

    2015-02-24

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

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

    EPA Science Inventory

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

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

    EPA Science Inventory

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

  15. X-RAY FLUORESCENCE ANALYSIS OF FILTER-COLLECTED AEROSOL PARTICLES

    EPA Science Inventory

    X-ray fluorescence (XRF) has become an effective technique for determining the elemental content of aerosol samples. For quantitative analysis, the aerosol particles must be collected as uniform deposits on the surface of Teflon membrane filters. An energy dispersive XRF spectrom...

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

    SciTech Connect

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

    1986-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    1992-11-01

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

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

    PubMed

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

    2015-02-24

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

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

    USGS Publications Warehouse

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

    1969-01-01

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

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

    SciTech Connect

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

    2015-02-24

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

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

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

  2. THE DEVELOPMENT OF POTENTIAL THIN STANDARDS FOR CALIBRATION OF X-RAY FLUORESCENCE SPECTROMETRY

    EPA Science Inventory

    Thin films containing known concentrations of metals are important for the calibration of X-ray Fluorescence Spectrometry (XRF), especially for the analysis of collected airborne particulate matter. A focused ion-beam sputtering technique has been investigated as a candidate meth...

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

    NASA Astrophysics Data System (ADS)

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

    2007-01-01

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

  4. SCANNING ELECTRON MICROSCOPY/X-RAY FLUORESCENCE CHARACTERIZATION OF POST-ABATEMENT DUST

    EPA Science Inventory

    Scanning electron microscopy (SEM) and laboratory X-ray fluorescence (XRF) were used to characterize post-abatement dust collected with a HEPA filtered vacuum. hree size fractions of resuspended dust (0-30 pm, 2.5-15 pm, and <2.5 pm) were collected on teflon filters and analyzed ...

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

    EPA Science Inventory

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

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

    ERIC Educational Resources Information Center

    Palmer, Peter T.

    2011-01-01

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

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

    SciTech Connect

    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.

  8. Experimental validation of L-shell x-ray fluorescence computed tomography imaging: phantom study.

    PubMed

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

    2015-10-01

    Thanks to the current advances in nanoscience, molecular biochemistry, and x-ray detector technology, x-ray fluorescence computed tomography (XFCT) has been considered for molecular imaging of probes containing high atomic number elements, such as gold nanoparticles. The commonly used XFCT imaging performed with K-shell x rays appears to have insufficient imaging sensitivity to detect the low gold concentrations observed in small animal studies. Low energy fluorescence L-shell x rays have exhibited higher signal-to-background ratio and appeared as a promising XFCT mode with greatly enhanced sensitivity. The aim of this work was to experimentally demonstrate the feasibility of L-shell XFCT imaging and to assess its achievable sensitivity. We built an experimental L-shell XFCT imaging system consisting of a miniature x-ray tube and two spectrometers, a silicon drift detector (SDD), and a CdTe detector placed at [Formula: see text] with respect to the excitation beam. We imaged a 28-mm-diameter water phantom with 4-mm-diameter Eppendorf tubes containing gold solutions with concentrations of 0.06 to 0.1% Au. While all Au vials were detectable in the SDD L-shell XFCT image, none of the vials were visible in the CdTe L-shell XFCT image. The detectability limit of the presented L-shell XFCT SDD imaging setup was 0.007% Au, a concentration observed in small animal studies. PMID:26839910

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

    NASA Astrophysics Data System (ADS)

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

    2016-06-01

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

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

    PubMed

    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 mm(3)) 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. PMID:27370459

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

    SciTech Connect

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

    2006-10-29

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

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

    SciTech Connect

    Wang, Xin

    1996-12-01

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

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

    SciTech Connect

    Manohar, Nivedh; Cho, Sang Hyun

    2014-10-15

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

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

    PubMed Central

    Manohar, Nivedh; Jones, Bernard L.; Cho, Sang Hyun

    2014-01-01

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

  15. Surface extended x-ray absorption fine structure of low-Z absorbates using fluorescence detection

    SciTech Connect

    Stoehr, J.; Kollin, E.B.; Fischer, D.A.; Hastings, J.B.; Zaera, F.; Sette, F.

    1985-05-01

    Comparison of x-ray fluorescence yield (FY) and electron yield surface extended x-ray absorption fine structure spectra above the S K-edge for c(2 x 2) S on Ni(100) reveals an order of magnitude higher sensitivity of the FY technique. Using FY detection, thiophene (C/sub 4/H/sub 4/S) chemisorption on Ni(100) is studied with S coverages down to 0.08 monolayer. The molecule dissociates at temperatures as low as 100K by interaction with fourfold hollow Ni sites. Blocking of these sites by oxygen leaves the molecule intact.

  16. SAVLOC, computer program for automatic control and analysis of X-ray fluorescence experiments

    NASA Technical Reports Server (NTRS)

    Leonard, R. F.

    1977-01-01

    A program for a PDP-15 computer is presented which provides for control and analysis of trace element determinations by using X-ray fluorescence. The program simultaneously handles data accumulation for one sample and analysis of data from previous samples. Data accumulation consists of sample changing, timing, and data storage. Analysis requires the locating of peaks in X-ray spectra, determination of intensities of peaks, identification of origins of peaks, and determination of a real density of the element responsible for each peak. The program may be run in either a manual (supervised) mode or an automatic (unsupervised) mode.

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

    PubMed

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

    2015-08-01

    This work evaluated the fluorescent dye degradation indirectly induced by ionizing radiation with high energy photons (50 keV). Aqueous gels of agarose with low concentrations of Rhodamine 6G and Fluorescein were submitted to doses of x-ray radiation up to 200 Gy. The dye degradation was analyzed by fluorescence spectroscopy, using an excitation light-emitting diode with a peak wavelength of 462 nm. A rate equation model of fluorophores and radicals' species populations was developed to describe the degradation time behavior of the fluorescent solutions. The model suggests fluorescent dyes should be used in dosimetry. PMID:26368112

  18. X-ray fluorescence microtomography of SiC shells

    SciTech Connect

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

    1997-04-01

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

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

    PubMed Central

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

    2016-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  1. New Approaches for Correction of Interlayer Absorption Effects in X-ray Fluorescence Imaging of Paintings.

    PubMed

    Wróbel, Paweł M; Frączek, Piotr; Lankosz, Marek

    2016-02-01

    The X-ray fluorescence imaging technique allows not only the imaging itself but also the identification of the hidden paint layers what makes it much more versatile as compared with X-ray radiography. One of the main disadvantages of the former method is the fact that the characteristic X-rays from the deeper paint layers are absorbed in the covering layers. This effect is manifested by some artifacts that impede a proper interpretation of the acquired images. In this work, it is shown that the methodology for correction of the interlayer absorption effects can be extended to the case of polychromatic excitation. Additionally, a new approach for determination of the optimal correction parameters has also been presented. The methodology was verified using either the test painting or the mock-up painting both measured with a table-top micro-XRF setup. PMID:26708500

  2. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    SciTech Connect

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang Rong

    2007-01-19

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  3. Optimizing Monocapillary Optics for Synchrotron X-ray Diffraction, Fluorescence Imaging, and Spectroscopy Applications

    NASA Astrophysics Data System (ADS)

    Bilderback, Donald H.; Kazimirov, Alexander; Gillilan, Richard; Cornaby, Sterling; Woll, Arthur; Zha, Chang-Sheng; Huang, Rong

    2007-01-01

    A number of synchrotron x-ray applications such as powder diffraction in diamond anvil cells, microbeam protein crystallography, x-ray fluorescence imaging, etc. can benefit from using hollow glass monocapillary optics to improve the flux per square micron on a sample. We currently draw glass tubing into the desired elliptical shape so that only one-bounce under total reflection conditions is needed to bring the x-ray beam to a focus at a 25 to 50 mm distance beyond the capillary tip. For modest focal spot sizes of 10 to 20 microns, we can increase the intensity per square micron by factors of 10 to 1000. We show some of the results obtained at CHESS and Hasylab with capillaries focusing 5 to 40 keV radiation, their properties, and how even better the experimental results could be if more ideal capillaries were fabricated in the future.

  4. Reference-free total reflection X-ray fluorescence analysis of semiconductor surfaces with synchrotron radiation.

    PubMed

    Beckhoff, Burkhard; Fliegauf, Rolf; Kolbe, Michael; Müller, Matthias; Weser, Jan; Ulm, Gerhard

    2007-10-15

    Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed. PMID:17880182

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

    NASA Astrophysics Data System (ADS)

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

    NASA Astrophysics Data System (ADS)

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

    2016-02-01

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

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

    PubMed

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

    2016-03-01

    X-ray fluorescence (XRF) analysis is one of the standard tools for the analysis of stratified materials and is widely applied for the investigation of electronics and coatings. The composition and thickness of the layers can be determined quantitatively and non-destructively. Recent work showed that these capabilities can be extended towards retrieving stratigraphic information like concentration depth profiles using angle-resolved XRF (ARXRF). This paper introduces an experimental sample chamber which was developed as a multi-purpose tool enabling different measurement geometries suited for transmission measurements, conventional XRF, ARXRF, etc. The chamber was specifically designed for attaching all kinds of laboratory X-ray sources for the soft and hard X-ray ranges as well as various detection systems. In detail, a setup for ARXRF using an X-ray tube with a polycapillary X-ray lens as source is presented. For such a type of setup, both the spectral and lateral characterizations of the radiation field are crucial for quantitative ARXRF measurements. The characterization is validated with the help of a stratified validation sample. PMID:27036820

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

    PubMed Central

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

    2013-01-01

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

  9. X-ray fluorescence from the element with atomic number Z=120.

    PubMed

    Frégeau, M O; Jacquet, D; Morjean, M; Bonnet, E; Chbihi, A; Frankland, J D; Rivet, M F; Tassan-Got, L; Dechery, F; Drouart, A; Nalpas, L; Ledoux, X; Parlog, M; Ciortea, C; Dumitriu, D; Fluerasu, D; Gugiu, M; Gramegna, F; Kravchuk, V L; Marchi, T; Fabris, D; Corsi, A; Barlini, S

    2012-03-23

    An atomic clock based on x-ray fluorescence yields has been used to estimate the mean characteristic time for fusion followed by fission in reactions 238U + 64Ni at 6.6  MeV/A. Inner shell vacancies are created during the collisions in the electronic structure of the possibly formed Z=120 compound nuclei. The filling of these vacancies accompanied by a x-ray emission with energies characteristic of Z=120 can take place only if the atomic transitions occur before nuclear fission. Therefore, the x-ray yield characteristic of the united atom with 120 protons is strongly related to the fission time and to the vacancy lifetimes. K x rays from the element with Z=120 have been unambiguously identified from a coupled analysis of the involved nuclear reaction mechanisms and of the measured photon spectra. A minimum mean fission time τ(f)=2.5×10(-18)  s has been deduced for Z=120 from the measured x-ray multiplicity. PMID:22540578

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

    PubMed

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

    2014-08-19

    Synchrotron radiation X-ray fluorescence (SR-XRF) is a powerful elemental analysis tool, yet synchrotrons are large, multiuser facilities that are generally not amenable to modification. However, the X-ray beamlines from synchrotrons can be modified by simply including X-ray filters or removing monochromators to improve the SR-XRF analysis. In this study, we evaluated four easily applied beamline configurations for the analysis of three representative environmental samples, namely a thin aerosol sample, an intermediate thickness biological sample, and a thick rare earth mineral specimen. The results showed that the "white beam" configuration, which was simply the full, polychromatic output of the synchrotron, was the optimal configuration for the analysis of thin samples with little mass. The "filtered white beam" configuration removed the lower energy X-rays from the excitation beam so it gave better sensitivity for elements emitting more energetic X-rays. The "filtered white beam-filtered detector" configuration sacrifices the lower energy part of the spectrum (<15 keV) for improved sensitivity in the higher end (∼26 to 48 keV range). The use of a monochromatic beam, which tends to be the standard mode of operation for most SR-XRF analyses reported in the literature, gave the least sensitive analysis. PMID:25025342

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

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

    SciTech Connect

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

    1997-04-01

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

  13. [Application of Three Dimensional Confocal Micro X-Ray Fluorescence Technology Based on Polycapillary X-Ray Lens in Analysis of Rock and Mineral Samples].

    PubMed

    Li, Fang-zuo; Liu, Zhi-guo; Sun, Tian-xi; Yi, Long-tao; Zhao, Wei-gang; He, Jia-lin; Peng, Song; Wang, Li-li; Zhao, Guang-cui; Ding, Xun-liang

    2015-09-01

    Confocal three dimensional (3D) micro X-ray fluorescence (XRF) spectrometer based on a polycapillary focusing X-ray lens (PFXRL) in the excitation channel and a polycapillary parallel X-ray lens (PPXRL) in the detection channel was developed. The PFXRL and PPXRL were placed in a confocal configuration. This was helpful in improving the signal-to-noise ratio of the XRF spectra, and accordingly lowered the detection limitation of the XRF technology. The confocal configuration ensured that only the XRF signal from the confocal micro-volume overlapped by the output focal spot of the PFXRL and the input focal spot of the PPXRL could be detected by the detector. Therefore, the point-to-point information of XRF for samples could be obtained non-destructively by moving the sample located at the confocal position. The magnitude of the gain in power density of the PFXRL was 10(3). This let the low power conventional X-ray source be used in this confocal XRF, and, accordingly, decreased the requirement of high power X-ray source for the confocal XRF based on polycapillary X-ray optics. In this paper, we used the confocal 3D micro X-ray fluorescence spectrometer to non-destructively analyzed mineral samples and to carry out a 3D point-to-point elemental mapping scanning, which demonstrated the capabilities of confocal 3D micro XRF technology for non-destructive analysis elements composition and distribution for mineral samples. For one mineral sample, the experimental results showed that the area with high density of element of iron had high density of copper. To some extent, this reflected the growth mechanisms of the mineral sample. The confocal 3D micro XRF technology has potential applications in such fields like the analysis identification of ore, jade, lithoid utensils, "gamble stone" and lithoid flooring. PMID:26669153

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

    NASA Astrophysics Data System (ADS)

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

    2003-12-01

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

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

    PubMed Central

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

    2014-01-01

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

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

    SciTech Connect

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

    2014-12-15

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

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

    SciTech Connect

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

    2015-01-01

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

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

    DOE PAGESBeta

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

    2015-01-01

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

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

    PubMed Central

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

    2016-01-01

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

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

    SciTech Connect

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

    2010-06-23

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

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

    SciTech Connect

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

    2009-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

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

    SciTech Connect

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

    1997-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-12-01

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

  6. X-ray Fluorescence Emission Tomography (XFET) with Novel Imaging Geometries – A Monte Carlo Study

    PubMed Central

    Meng, L. J.; Li, Nan; La Riviere, P. J.

    2011-01-01

    This paper presents a feasibility study for using two new imaging geometries for synchrotron X-ray fluorescence emission tomography (XFET) applications. In the proposed approaches, the object is illuminated with synchrotron X-ray beams of various cross-sectional dimensions. The resultant fluorescence photons are detected by high-resolution imaging-spectrometers coupled to collimation apertures. To verify the performance benefits of the proposed methods over the conventional line-by-line scanning approach, we have used both Monte Carlo simulations and an analytical system performance index to compare several different imaging geometries. This study has demonstrated that the proposed XFET approach could lead to a greatly improved imaging speed, which is critical for making XFET a practical imaging modality for a wide range of applications. PMID:22228913

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

    SciTech Connect

    Arp, U.; LeBrun, T.; Southworth, S.H.; Jung, M.; MacDonald, M.A.

    1996-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2008-12-01

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

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

    SciTech Connect

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

    1995-05-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  12. Cosputtered composition-spread reproducibility established by high-throughput x-ray fluorescence

    SciTech Connect

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

    2010-09-15

    We describe the characterization of sputtered yttria-zirconia composition spread thin films by x-ray fluorescence (XRF). We also discuss our automated analysis of the XRF data, which was collected in a high throughput experiment at the Cornell High Energy Synchrotron Source. The results indicate that both the composition reproducibility of the library deposition and the composition measurements have a precision of better than 1 atomic percent.

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

    SciTech Connect

    Glenn Moore

    2013-09-01

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

  14. Applications of synchrotron x-ray fluorescence microprobe techniques to photochromic materials

    SciTech Connect

    Perry, D.L.

    1996-12-31

    Applications of synchrotron x-ray fluorescence microprobe techniques to photochromic materials are presented regarding dopant metal ions in the crystal matrices. Types of samples that are amenable to the technique will be discussed, along with sample format and experimental conditions. The chemical information that one can obtain from samples will be presented, and examples of copant contaminant studies in crystals will be given. New types of samples that are possible to study using this technique will be presented.

  15. Quantitative X-ray fluorescence analysis of As-Se glasses and films

    NASA Astrophysics Data System (ADS)

    Bordovskiĭ, G. A.; Marchenko, A. V.; Seregin, P. P.; Smirnova, N. N.; Terukov, E. I.

    2009-11-01

    The concentrations of arsenic and selenium in As100 - x Se x glassy alloys and related films have been determined by the X-ray fluorescence spectroscopy using the external standard technique. It is demonstrated that the proposed approach allows the compositions of As100 - x Se x glasses and films to be quantitatively determined with an accuracy of Δ x = ±0.02.

  16. Determining analyte concentrations in plutonium metal by x-ray fluorescence using a dried residue method

    NASA Astrophysics Data System (ADS)

    Worley, Christopher G.; Havrilla, George J.

    2000-07-01

    Accurately determining the concentration of certain elements in plutonium is of vital importance in manufacturing nuclear weapons. X-ray fluorescence (XRF) provides a means of obtaining this type of elemental information accurately, quickly, with high precision, and often with little sample preparation. In the present work, a novel method was developed to analyze the gallium concentration in plutonium samples using wavelength-dispersive XRF. A description of the analytical method will be discussed.

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

    PubMed

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

    2010-02-01

    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. PMID:20071757

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

    SciTech Connect

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

    2013-05-15

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

  19. In vivo X-ray fluorescence of lead in bone: review and current issues.

    PubMed Central

    Todd, A C; Chettle, D R

    1994-01-01

    Bone lead measurements can assess long-term lead dosimetry because the residence time of lead in bone is long. Bone lead measurements thus complement blood and plasma lead measurements, which reflect more short-term exposure. Although the noninvasive, in vivo measurement of lead in bone by X-ray fluorescence (XRF) has been under development since the 1970s, its use is still largely confined to research institutions. There are three principal methods used that vary both in the how lead X-rays are fluoresced and in which lead X-rays are fluoresced. Several groups have reported the independent development of in vivo measurement systems, the majority adopting the 109Cd K XRF method because of its advantages: a robust measurement, a lower detection limit (compared to 57Co K XRF), and a lower effective (radiation) dose (compared to L XRF) when calculated according to the most recent guidelines. These advantages, and the subsequent widespread adoption of the 109Cd method, are primarily consequences of the physics principles of the technique. This paper presents an explanation of the principles of XRF, a description of the practical measurement systems, a review of the human bone lead studies performed to date; and a discussion of some issues surrounding future application of the methods. Images p172-a PMID:8033846

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

    PubMed Central

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

    2016-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2007-02-01

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

  2. A new workflow for x-ray fluorescence tomography: MAPStoTomoPy

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-06-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

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

  5. Correlative imaging of live biological cells with a soft x-ray microscope and a fluorescence microscope

    NASA Astrophysics Data System (ADS)

    Kado, M.; Kishimoto, M.; Tamotsu, S.; Yasuda, K.; Aoyama, M.; Tone, S.; Shinohara, K.

    2016-01-01

    A laser-plasma soft X-ray microscope which is a combination of a highly intense laser-plasma soft X-ray source and a contact microscopy has been developed. We have proposed a correlative imaging method with the laser-plasma soft X-ray microscope and a fluorescence microscope to observe the same biological cells with the both microscopes at the same time. Live hydrated biological cells and cellular organelles have been observed with the correlative imaging method. Using the information of the cellular organelles obtained with the fluorescence microscope, inner structures obtained with the soft X-ray microscope are identified. Since the spatial resolution of the soft X-ray microscope is much higher than that of the fluorescence microscope, fine structures of the cellular organelles of the live biological cells have been visualized with the correlative imaging.

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

    PubMed

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

    2012-07-01

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

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

    PubMed

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

    2012-05-15

    Confocal micro-beam X-ray fluorescence microscope was constructed. The system was assembled from commercially available components - a low power X-ray tube source, polycapillary X-ray optics and silicon drift detector - controlled by an in-house developed LabVIEW software. A video camera coupled to optical microscope was utilized to display the area excited by X-ray beam. The camera image calibration and scan area definition software were also based entirely on LabVIEW code. Presently, the main area of application of the newly constructed spectrometer is 2-dimensional mapping of element distribution in environmental, biological and geological samples with micrometer spatial resolution. The hardware and the developed software can already handle volumetric 3-D confocal scans. In this work, a front panel graphical user interface as well as communication protocols between hardware components were described. Two applications of the spectrometer, to homogeneity testing of titanium layers and to imaging of various types of grains in air particulate matter collected on membrane filters, were presented. PMID:22483897

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

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques. PMID:21615981

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

    NASA Astrophysics Data System (ADS)

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

    2014-02-01

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

  10. Effect of regolith on planetary X-ray fluorescence spectroscopy: laboratory and numerical studies

    NASA Astrophysics Data System (ADS)

    Naranen, Jyri; Carpenter, James; Parviainen, Hannu; Muinonen, Karri

    Fluorescent X-rays from the surfaces of airless planetary bodies in the inner solar system have been measured by instruments on several spacecraft. X-ray emission follows photoionisation by incident solar X-rays and charged particles and reveals the elemental composition of the surface. Analyses of X-ray spectra obtained by orbiting spacecraft, use the relative intensities of elemental emission lines (e.g., Ca/Si, Fe/Si) to determine the geochemistry of the target body. Historically, the analysis of X-ray spectra has assumed that surfaces can be considered as homogeneous plane-parallel media. It has been shown, however, that relative line intensities are affected by the physical properties of the target surface (e.g. particle size distribution and packing density of the regolith) and the viewing and illumination geometry of observations. We describe experimental investigations into the effects of regolith properties on the line ratios measured by a nadir pointing (emergence angle 0° ) orbiting instrument, with with solar illumination angles in the range 25-75° from zenith. The planetary regolith analogue used in these experiments was a terrestrial, olivine rich basalt, which has been used by previous authors as an analogue to the lunar maria. The basalt samples were ground to powder and sieved to discriminate particles in the ranges, <75µm, 75-250µm, and 250-500µm. These separate powders were then pressed into solid pellets. The separation of particles with different sizes allows some determination of the effects due to changes in particle size. All measurements were made at pressures of less than 0.5 mbar to prevent absorption of fluorescent X-rays in air. The relative fluorescent line ratios of several major rock forming elements (K, Ca, Ti, Si) were measured. We find that for measurements made in a "nadir" pointing geometry, the measured spectrum becomes increasingly hard as illumination angle increases (i.e. X-ray lines at higher energies are enhanced

  11. STANDARD OPERATING PROCEDURES FOR MEASUREMENT OF LEAD IN PAINT USING THE SCITEC MAP-3 X-RAY FLUORESCENCE SPECTROMETER

    EPA Science Inventory

    A portable X-ray fluorescence (XRF) procedure for quantatively measuring lead in paint in situ is described along with recommended QA/QC practices. he procedure was evaluated using calibration paint films over various substrates and with field samples. sing the K shell X-rays, a ...

  12. Multispectral pattern recognition applied to x-ray fluorescence images of the Archimedes Palimpsest

    NASA Astrophysics Data System (ADS)

    Hansen, D. Michael; Easton, Roger L., Jr.; Raqueño, Rolando

    2007-01-01

    The Archimedes Palimpsest is one of the most significant texts in the history of science. Much of the text has been read using images of reflected visible light and visible light produced by ultraviolet fluorescence. However, these techniques do not perform well on the four pages of the manuscript that are obscured by forged icons that were painted over these pages during the first half of the 20th century. X-ray fluorescence images of one of these pages have been processed using spectral pattern recognition techniques developed for environmental remote sensing to recover the original texts beneath the paint.

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

    SciTech Connect

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

    1997-04-01

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

  14. Feasibility study for the in vivo measurement of lead in bone using L-x-ray fluorescence

    SciTech Connect

    Wielopolski, L.; Slatkin, D.N.; Vartsky, D.; Ellis, K.J.; Cohn, S.H.

    1980-01-01

    Lead deposits in bone were detected by x-ray fluorescence using x-rays from either a /sup 125/I or a /sup 109/Cd source. Measurements were taken from tibia in intact human legs, post-mortem. On the basis of preliminary measurements, it was concluded that an exposure of one rad is adequate for determination of lead in bone. Both the advantages and the disadvantages of L-x-rays, used in the technique developed for this study, are compared with those of K-x-rays.

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

    SciTech Connect

    Havrilla, George J; Collins, Michael L; Montoya, Velma M; Chen, Zewu; Wei, Fuzhong

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

    PubMed

    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. PMID:23576194

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

    NASA Astrophysics Data System (ADS)

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

    2014-03-01

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

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

    SciTech Connect

    Grodzins, Lee; Niland, John

    2002-05-23

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

  19. Spontaneous soft x-ray fluorescence from a superlattice under Kossel diffraction conditions

    NASA Astrophysics Data System (ADS)

    Jonnard, P.; Yuan, Y.-Y.; Le Guen, K.; André, J.-M.; Zhu, J.-T.; Wang, Z.-S.; Bridou, F.

    2014-08-01

    The present study gives the proof of principle of a technique that is an extension of Kossel diffraction both from crystals to superlattices and toward the soft x-ray region, allowing the characterization of the interfaces within a periodic structure. We measure the intensity of the Co Lα and Mg Kα characteristic fluorescence emissions from a Mg/Co superlattice upon soft x-ray excitation. The observation is made so that the angle between the sample surface and the detection direction is scanned around the first and second Bragg peaks of the fluorescence emissions. Clear modulations of the emitted intensities are observed and well reproduced by simulations based on the reciprocity theorem and assuming a perfect stack. The present work gives evidence that such a superlattice plays the role of an optical cavity for the spontaneous emission generated within the stack. This should also be the case for stimulated emission, which when combined with pumping free electron laser, will open the road to innovative x-ray distributed feedback lasers.

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

    SciTech Connect

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

    2009-01-01

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

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

    DOEpatents

    Wilson, Bary W.; Shepard, Chester L.

    2005-02-22

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

  2. Simultaneous x-ray nano-ptychographic and fluorescence microscopy at the bionanoprobe

    NASA Astrophysics Data System (ADS)

    Chen, S.; Deng, J.; Vine, D. J.; Nashed, Y. S. G.; Jin, Q.; Peterka, T.; Jacobsen, C.; Vogt, S.

    2015-09-01

    Hard X-ray fluorescence (XRF) microscopy offers unparalleled sensitivity for quantitative analysis of most of the trace elements in biological samples, such as Fe, Cu, and Zn. These trace elements play critical roles in many biological processes. With the advanced nano-focusing optics, nowadays hard X-rays can be focused down to 30 nm or below and can probe trace elements within subcellular compartments. However, XRF imaging does not usually reveal much information on ultrastructure, because the main constituents of biomaterials, i.e. H, C, N, and O, have low fluorescence yield and little absorption contrast at multi-keV X-ray energies. An alternative technique for imaging ultrastructure is ptychography. One can record far-field diffraction patterns from a coherently illuminated sample, and then reconstruct the complex transmission function of the sample. In theory the spatial resolution of ptychography can reach the wavelength limit. In this manuscript, we will describe the implementation of ptychography at the Bionanoprobe (a recently developed hard XRF nanoprobe at the Advanced Photon Source) and demonstrate simultaneous ptychographic and XRF imaging of frozen-hydrated biological whole cells. This method allows locating trace elements within the subcellular structures of biological samples with high spatial resolution. Additionally, both ptychographic and XRF imaging are compatible with tomographic approach for 3D visualization.

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

    PubMed

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

    2016-07-01

    An X-ray fluorescence flow cytometer that can determine the total metal content of single cells has been developed. Capillary action or pressure was used to load cells into hydrophilic or hydrophobic capillaries, respectively. Once loaded, the cells were transported at a fixed vertical velocity past a focused X-ray beam. X-ray fluorescence was then used to determine the mass of metal in each cell. By making single-cell measurements, the population heterogeneity for metals in the µM to mM concentration range on fL sample volumes can be directly measured, a measurement that is difficult using most analytical methods. This approach has been used to determine the metal composition of 936 individual bovine red blood cells (bRBC), 31 individual 3T3 mouse fibroblasts (NIH3T3) and 18 Saccharomyces cerevisiae (yeast) cells with an average measurement frequency of ∼4 cells min(-1). These data show evidence for surprisingly broad metal distributions. Details of the device design, data analysis and opportunities for further sensitivity improvement are described. PMID:27359138

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

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

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

    SciTech Connect

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

    2007-01-19

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

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

    NASA Astrophysics Data System (ADS)

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

    2007-09-01

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

  7. Equipment design issues for the in vivo X-ray fluorescence analysis of bone lead.

    PubMed Central

    Thomas, B J

    1991-01-01

    Several groups have reported the development of systems, based on the principle of X-ray fluorescence, for the in vivo measurement of bone lead concentrations. These systems have used the detection of either the characteristic L or K X-rays resulting from excitation by a suitable photon source. This paper examines design issues related to the development of these systems. These design issues are, in most instances, a result of consideration of the physical principles involved, and hence there are many features common to the systems developed by the individual groups. Design issues discussed in this paper include the selection of the site for measurement, source-sample-detector configuration, and collimation. Specific examples from published work are used to demonstrate the relevant features. PMID:2040249

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

    USGS Publications Warehouse

    Taggart, Joseph E.

    1985-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2013-07-01

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

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

    SciTech Connect

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

    2011-07-06

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

  11. Fluorescent X-Ray Computed Tomography towards Molecular Imaging: Proof-of-Concept Experiments

    SciTech Connect

    Yuasa, Tetsuya; Huo, Qingkai; Akatsuka, Takao; Takeda, Tohoru; Hyodo, Kazuyuki; Dilmanian, F. Avraham

    2009-03-10

    By means of fluorescent x-ray computed tomography (FXCT) one can detect and image a distribution of non-radioactive imaging agent, e.g., iodine, in a biomedical subject at a high spatial resolution, so it can be a novel molecular imaging modality. We have been studying an FXCT system using synchrotron radiation for in-vivo imaging brains of small animals such as mouse, or rat. For the purpose, we propose a fast FXCT imaging method based on the novel geometry. In this study, we prove the feasibility of this concept and investigate its imaging properties, including spatial and contrast resolutions and quantitativeness, by imaging an acrylic phantom and a normal mouse brain using a preliminary imaging system with monochromatic synchrotron x rays.

  12. Quantitative time-averaged gas and liquid distributions using x-ray fluorescence and radiography in atomizing sprays.

    PubMed

    Radke, Christopher D; McManamen, J Patrick; Kastengren, Alan L; Halls, Benjamin R; Meyer, Terrence R

    2015-05-01

    A method for quantitative measurements of gas and liquid distributions is demonstrated using simultaneous x-ray fluorescence and radiography of both phases in an atomizing coaxial spray. Synchrotron radiation at 10.1 keV from the Advanced Photon Source at Argonne National Laboratory is used for x-ray fluorescence of argon gas and two tracer elements seeded into the liquid stream. Simultaneous time-resolved x-ray radiography combined with time-averaged dual-tracer fluorescence measurements enabled corrections for reabsorption of x-ray fluorescence photons for accurate, line-of-sight averaged measurements of the distribution of the gas and liquid phases originating from the atomizing nozzle. PMID:25927776

  13. AUTOMATIC PARTICULATE SULFUR MEASUREMENTS WITH A DICHOTOMOUS SAMPLER AND ON-LINE X-RAY FLUORESCENCE ANALYSIS

    EPA Science Inventory

    An instrument is described which employs a dichotomous sampler to acquire fine particulate samples on a continuous tape filter. Analyses for elemental sulfur are performed immediately following acquisition using a sensitive X-ray fluorescence spectrometer. Sample sequencing, data...

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

    PubMed

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

    2012-02-01

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

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

    PubMed Central

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

    2012-01-01

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

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

    SciTech Connect

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

    2015-05-15

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

  17. Several approaches to the investigation of paintings with the use of portable X-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Trojek, T.; Trojková, D.

    2015-11-01

    This paper deals with several approaches to the application of X-ray fluorescence analysis and micro-analysis to non-destructive investigations of paintings. The methodology is described and demonstrated on a painting of known structure that was painted with modern artistic tempera paints. There is also a description and a demonstration of three depth profiling techniques that provide information on the depth distribution of elements in the surface layers of a painting. The three techniques utilize (a) the internal X-ray ratios of the elements that are present, (b) X-ray fluorescence analysis with two detectors with different angles of detection of characteristic X-rays, and (c) a technique based on comparing X-ray spectra measured with a tilted sample. The capabilities and demands on instrumentation and interpretation of the results are compared for all these techniques.

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

    PubMed

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

    2015-05-01

    A new multipurpose x-ray reflectometer station has been developed and augmented at the microfocus beamline (BL-16) of Indus-2 synchrotron radiation source to facilitate synchronous measurements of specular x-ray reflectivity and grazing incidence x-ray fluorescence emission from thin layered structures. The design and various salient features of the x-ray reflectometer are discussed. The performance of the reflectometer has been evaluated by analyzing several thin layered structures having different surface interface properties. The results reveal in-depth information for precise determination of surface and interface properties of thin layered materials demonstrating the immense potential of the combined measurements of x-ray reflectivity and grazing incidence fluorescence on a single reflectometer. PMID:26026553

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

    SciTech Connect

    Worley, Christopher G

    2009-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2009-04-01

    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 Kα1 and Kβ1 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 well

  1. Hyper-filter-fluorescer spectrometer for x-rays above 120 keV

    DOEpatents

    Wang, Ching L.

    1983-01-01

    An apparatus utilizing filter-fluorescer combinations is provided to measure short bursts of high fluence x-rays above 120 keV energy, where there are no practical absorption edges available for conventional filter-fluorescer techniques. The absorption edge of the prefilter is chosen to be less than that of the fluorescer, i.e., E.sub.PRF E.sub.F. In this way, the response function is virtually zero between E.sub.PRF and E.sub.F and well defined and enhanced in an energy band of less than 1000 keV above the 120 keV energy.

  2. Fast X-Ray Fluorescence Camera Combined with Wide Band Pass Monochromatic Synchrotron Beam

    SciTech Connect

    Sakurai, Kenji; Mizusawa, Mari

    2004-05-12

    A double W/B4C multilayer monochromator (2d=50.4A) was commissioned for non-scanning X-ray fluorescence (XRF) imaging experiments. The combination of a brilliant multi-pole wiggler source and the present wide band pass monochromator permits 1.2 x 1013 photons/sec at the sample position for 8.04 keV X-rays. Energy resolution {delta}E and {delta}E/E are 300{approx}500 eV and {approx}5%, respectively. The exit beam height is constant for X-ray energy ranging from 5.5 to 13.0 keV. Indirect cooling of the 1st multilayer works successfully. In addition, a new fast CCD camera was developed for quick readout and transfer of the image data. It was found that the typical exposure time for one XRF image with 1000 x 1000 pixels is 0.03{approx}1 sec. This permits in-situ movie recording for the distribution of elements.

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

    SciTech Connect

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

    2010-10-14

    Phase-resolved x-ray ferromagnetic resonance (XFMR) has been measured in fluorescence yield, extending the application of XFMR to opaque samples on opaque substrates. Magnetization dynamics were excited in a Co{sub 50}Fe{sub 50}(0.7)/Ni{sub 90}Fe{sub 10}(5) bilayer by means of a continuous wave microwave excitation, while x-ray magnetic circular dichroism (XMCD) spectra were measured stroboscopically at different points in the precession cycle. By tuning the x-ray energy to the L{sub 3} edges of Ni and Fe, the dependence of the real and imaginary components of the element specific magnetic susceptibility on the strength of an externally applied static bias field was determined. First results from measurements on a Co{sub 50}Fe{sub 50}(0.7)/Ni{sub 90}Fe{sub 10}(5)/Dy(1) sample confirm that enhanced damping results from the addition of the Dy cap.

  4. Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.

    1989-01-01

    Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

  5. Development of Ta-based Superconducting Tunnel Junction X-ray Detectors for Fluorescence XAS

    SciTech Connect

    Friedrich, S; Drury, O; Hall, J; Cantor, R

    2009-09-23

    We are developing superconducting tunnel junction (STJ) soft X-ray detectors for chemical analysis of dilute samples by fluorescence-detected X-ray absorption spectroscopy (XAS). Our 36-pixel Nb-based STJ spectrometer covers a solid angle {Omega}/4{pi} {approx} 10{sup -3}, offers an energy resolution of {approx}10-20 eV FWHM for energies up to {approx}1 keV, and can be operated at total count rates of {approx}10{sup 6} counts/s. For increased quantum efficiency and cleaner response function, we have now started the development of Ta-based STJ detector arrays. Initial devices modeled after our Nb-based STJs have an energy resolution below 10 eV FWHM for X-ray energies below 1 keV, and pulse rise time discrimination can be used to improve their response function for energies up to several keV. We discuss the performance of the Ta-STJs and outline steps towards the next-generation of large STJ detector arrays with higher sensitivity.

  6. Development of Ta-based Superconducting Tunnel Junction X-ray Detectors for Fluorescence XAS

    SciTech Connect

    Friedrich, Stephan; Drury, Owen B.; Hall, John; Cantor, Robin

    2010-06-23

    We are developing superconducting tunnel junction (STJ) soft X-ray detectors for chemical analysis of dilute samples by fluorescence-detected X-ray absorption spectroscopy (XAS). Our 36-pixel Nb-based STJ spectrometer covers a solid angle {Omega}/4{pi}{approx_equal}10{sup -3}, offers an energy resolution of {approx}10-20 eV FWHM for energies up to {approx}1 keV, and can be operated at total count rates of {approx}10{sup 6} counts/s. For increased quantum efficiency and cleaner response function, we have now started the development of Ta-based STJ detector arrays. Initial devices modeled after our Nb-based STJs have an energy resolution below 10 eV FWHM for X-ray energies below 1 keV, and pulse rise time discrimination can be used to improve their response function for energies up to several keV. We discuss the performance of the Ta-STJs and outline steps towards the next-generation of large STJ detector arrays with higher sensitivity.

  7. Proton-induces and x-ray induced fluorescence analysis of scoliotic tissue

    SciTech Connect

    Panessa-Warren, B J; Kraner, H W; Jones, K W; Weiss, L S

    1980-02-01

    Adolescent idiopathic scoliosis is characterized by a curvature or assymetry of the spine which may become progressively more severe, with clinical symptoms appearing just prior to, or during, puberty. The incidence for scoliosis in the age group from 12 to 14 years of age has been reported as high as 8 to 10%, with more than 80% of the cases occurring in females. Although pathologic changes exist in muscles from both sides of the spinal curvature, and no statistically significant side differences have been reported, morphologic changes suggest that the concanve side is the most affected. This paper reports our preliminary data on the elemental composition of individual muscle fibers derived from convex, concave and gluteal scoliotic muscle, and erythrocytes from scoliotic and normal patients, analyzed by proton induced x-ray emission (PIXE) and x-ray fluorescence spectroscopy (XRF). A new type of specimen holder was designed for this study which offers low x-ray background, minimal absorption and maintenance of a moist environment around the specimen.

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

    NASA Astrophysics Data System (ADS)

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

    2009-09-01

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

  9. X-ray fluorescence analysis of iron and manganese distribution in primary dopaminergic neurons

    PubMed Central

    Dučić, Tanja; Barski, Elisabeth; Salome, Murielle; Koch, Jan C; Bähr, Mathias; Lingor, Paul

    2013-01-01

    Transition metals have been suggested to play a pivotal role in the pathogenesis of Parkinson's disease. X-ray microscopy combined with a cryogenic setup is a powerful method for elemental imaging in low concentrations and high resolution in intact cells, eliminating the need for fixation and sectioning of the specimen. Here, we performed an elemental distribution analysis in cultured primary midbrain neurons with a step size in the order of 300 nm and ∼ 0.1 ppm sensitivity under cryo conditions by using X-ray fluorescence microscopy. We report the elemental mappings on the subcellular level in primary mouse dopaminergic (DAergic) and non-DAergic neurons after treatment with transition metals. Application of Fe2+ resulted in largely extracellular accumulation of iron without preference for the neuronal transmitter subtype. A quantification of different Fe oxidation states was performed using X-ray absorption near edge structure analysis. After treatment with Mn2+, a cytoplasmic/paranuclear localization of Mn was observed preferentially in DAergic neurons, while no prominent signal was detectable after Mn3+ treatment. Immunocytochemical analysis correlated the preferential Mn uptake to increased expression of voltage-gated calcium channels in DAergic neurons. We discuss the implications of this differential elemental distribution for the selective vulnerability of DAergic neurons and Parkinson's disease pathogenesis. PMID:23106162

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

    PubMed

    Li, Fang; Wang, Ji-hua; Lu, An-xiang; Han, Ping

    2015-04-01

    The concentration of Cr, Cu, Zn, As and Pb in soil was tested by portable X-ray fluorescence spectrometer. Each sample was tested for 3 times, then after using wavelet threshold noise filtering method for denoising and smoothing the spectra, a standard curve for each heavy metal was established according to the standard values of heavy metals in soil and the corresponding counts which was the average of the 3 processed spectra. The signal to noise ratio (SNR), mean square error (MSE) and information entropy (H) were taken to assess the effects of denoising when using wavelet threshold noise filtering method for determining the best wavelet basis and wavelet decomposition level. Some samples with different concentrations and H3 B03 (blank) were chosen to retest this instrument to verify its stability. The results show that: the best denoising result was obtained with the coif3 wavelet basis at the decomposition level of 3 when using the wavelet transform method. The determination coefficient (R2) range of the instrument is 0.990-0.996, indicating that a high degree of linearity was found between the contents of heavy metals in soil and each X-ray fluorescence spectral characteristic peak intensity with the instrument measurement within the range (0-1,500 mg · kg(-1)). After retesting and calculating, the results indicate that all the detection limits of the instrument are below the soil standards at national level. The accuracy of the model has been effectively improved, and the instrument also shows good precision with the practical application of wavelet transform to the establishment and improvement of X-ray fluorescence spectrometer detection model. Thus the instrument can be applied in on-site rapid screening of heavy metal in contaminated soil. PMID:26197612

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

    SciTech Connect

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

    2012-03-13

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

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

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

    NASA Astrophysics Data System (ADS)

    Liu, Jiren

    2016-06-01

    X-ray fluorescent lines are unique features of the reflection spectrum of the torus when irradiated by the central active galactic nuclei (AGN). Their intrinsic line width can be used to probe the line-emitting region. Previous studies have focused on the Fe K α 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 ˜1860 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 K α line is located. We measured the full width at half-maximum of the Si K α line for Circinus, Mrk 3, and NGC 1068, which are 570 ± 240, 730 ± 320, and 320 ± 280 km s-1, respectively. They are 3-5 times smaller than those measured with the Fe K α line previously. It shows that the intrinsic widths of the Fe K α line are most likely to be overestimated. The measured widths of the Si K α line put the line-emitting region outside the dust sublimation radius in these galaxies. It indicates that for Compton-thick AGN, the X-ray fluorescence material are likely to be the same as the dusty torus emitting in the infrared band.

  14. The Bionanoprobe: hard X-ray fluorescence nanoprobe with cryogenic capabilities

    PubMed Central

    Chen, S.; Deng, J.; Yuan, Y.; Flachenecker, C.; Mak, R.; Hornberger, B.; Jin, Q.; Shu, D.; Lai, B.; Maser, J.; Roehrig, C.; Paunesku, T.; Gleber, S. C.; Vine, D. J.; Finney, L.; VonOsinski, J.; Bolbat, M.; Spink, I.; Chen, Z.; Steele, J.; Trapp, D.; Irwin, J.; Feser, M.; Snyder, E.; Brister, K.; Jacobsen, C.; Woloschak, G.; Vogt, S.

    2014-01-01

    Hard X-ray fluorescence microscopy is one of the most sensitive techniques for performing trace elemental analysis of biological samples such as whole cells and tissues. Conventional sample preparation methods usually involve dehydration, which removes cellular water and may consequently cause structural collapse, or invasive processes such as embedding. Radiation-induced artifacts may also become an issue, particularly as the spatial resolution increases beyond the sub-micrometer scale. To allow imaging under hydrated conditions, close to the ‘natural state’, as well as to reduce structural radiation damage, the Bionanoprobe (BNP) has been developed, a hard X-ray fluorescence nanoprobe with cryogenic sample environment and cryo transfer capabilities, dedicated to studying trace elements in frozen-hydrated biological systems. The BNP is installed at an undulator beamline at sector 21 of the Advanced Photon Source. It provides a spatial resolution of 30 nm for two-dimensional fluorescence imaging. In this first demonstration the instrument design and motion control principles are described, the instrument performance is quantified, and the first results obtained with the BNP on frozen-hydrated whole cells are reported. PMID:24365918

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

    NASA Astrophysics Data System (ADS)

    Rousseau, Richard M.

    2006-07-01

    This paper presents the basic concepts of the mathematical correction for matrix effects in X-ray fluorescence analysis. The emphasis is placed on the correction factor for matrix effects and its quantification. This correction factor is calculated using mathematical models proposed by Lachance-Traill, Claisse-Quintin and Rousseau, which can be applied in practice via an efficient calibration procedure. Each variable in these models is clearly identified so that specific numerical values can easily be substituted for calculation. This paper describes and emphasizes the application of the most effective existing models.

  16. Analysis of obsidian artifacts in Southern Meso-America using x-ray fluorescence

    SciTech Connect

    Nelson, F.W.

    1996-12-31

    The analysis of obsidian artifacts using X-ray fluorescence (XRF) spectrometry has been an important tool for archaeologists for {approximately}25 yr. However, as methods and instrumentation have improved, more reliable information regarding exchange and routes of exchange has been obtained. In southern Meso-America, obsidian analyses have demonstrated changes in the obsidian geologic sources used by prehistoric peoples through time. These changes in sources of obsidian have been used to describe possible changes of prehistoric trade routes. The methods and results of analysis are described in this paper.

  17. Preliminary testing of a prototype portable X-ray fluorescence spectrometer

    NASA Technical Reports Server (NTRS)

    Patten, L. L.; Anderson, N. B.; Stevenson, J. J.

    1982-01-01

    A portable X-ray fluorescence spectrometer for use as an analyzer in mineral resource investigative work was built and tested. The prototype battery powered spectrometer, measuring 11 by 12 by 5 inches and weighing only about 15 pounds, was designed specifically for field use. The spectrometer has two gas proportional counters and two radioactive sources, Cd (10a) and Fe (55). Preliminary field and laboratory tests on rock specimens and rock pulps have demonstrated the capability of the spectrometer to detect 33 elements to date. Characteristics of the system present some limitations, however, and further improvements are recommended.

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

    NASA Astrophysics Data System (ADS)

    von Bohlen, Alex; Meyer, Friedrich

    1997-07-01

    Total reflection X-ray fluorescence was used to characterize elements (with Z>13) contained in varnishes applied by prominent violin makers during the last five centuries. Direct analyses of small flakes with masses <20 μg show a variety of elements. Some of these elements could be related to key elements of inorganic pigments and additives used to control some of the properties of a varnish. Higher amounts of Fe, As and Pb were found in old products, Mn, Co, Cu, Zn and Pb were used in more recent varnishes.

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

    SciTech Connect

    Worley, Christopher G; Sodweberg, Constance B; Townsend, Lisa E

    2009-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

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

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

    SciTech Connect

    Stojanoff, V.; Hamalainen, K.; Siddons, D.P.; Hastings, J.B.; Berman, L.E.; Cramer, S.; Smith, G.

    1991-01-01

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

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

    SciTech Connect

    Stojanoff, V.; Hamalainen, K.; Siddons, D.P.; Hastings, J.B.; Berman, L.E.; Cramer, S.; Smith, G.

    1991-12-31

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

  3. Synchrotron based X-ray fluorescence activities at Indus-2: An overview

    SciTech Connect

    Tiwari, M. K.

    2014-04-24

    X-Ray fluorescence (XRF) spectrometry is a powerful non-destructive technique for elemental analysis of materials at bulk and trace concentration levels. Taking into consideration several advantages of the synchrotron based XRF technique and to fulfill the requirements of Indian universities users we have setup a microfocus XRF beamline (BL-16) on Indus-2 synchrotron light source. The beamline offers a wide range of usages – both from research laboratories and industries; and for researchers working in diverse fields. A brief overview of the measured performance of the beamline, design specifications including various attractive features and recent research activities carried out on the BL-16 beamline are presented.

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

    SciTech Connect

    Alatas, A.; Alp, E. E.; Friedman, E. S.; Jennings, G.; Johnson, C. E.; Lai, B.; Mini, S. M.; Sato, Y.; Wilkinson, T. J.; Yener, K. A.

    1999-03-10

    Sediments from relic Lake Golbasi were analyzed by X-ray fluorescence with synchrotrons radiation to determine changes in element concentrations over time with selected elements serving as proxies for environmental change. Increases in Ca and Sr suggest soil formation during a dry period, from ca. 4500 BC to ca. 200 AD at which point K, Rb, Zr, Ti, and Y increase, indicating the return of a wet environment. Soil erosion, represented by Cr and Ni, increases ca. 7000 BC, probably as a consequence of environmental change, prior to suggested exploitation of natural resources by the newly urbanized society of the third millennium BC.

  5. Desert Varnish: Relative and Absolute Dating Using Portable X-Ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Pingitore, N. E.; Lytle, F. W.

    2003-12-01

    Levels of manganese and iron measured in situ with a portable x-ray fluorescence instrument permit relative and absolute dating of desert varnish. This novel technique may have wide potential application to dating Pleistocene and Holocene events and geomorphic surfaces in dry climate settings. Desert varnish is a thin biogenic coating, enriched in Mn and Fe, found on rock surfaces in arid and semi-arid regions. The accumulation of varnish marks the passage of time since a fresh rock surface was created or exposed. Thus the varnish thickness reflects the age of the event that created the fresh surface, whatever the agent was, e.g., a rock fall, a fault movement, or an aboriginal artist. Past attempts to date rock varnish have been marked more by ambiguity or outright failure than by success. Our recent research suggests a practical and rapid method for dating varnish using a portable x-ray fluorescence instrument (PXRF). Varnish thickness encodes two distinct signals, metal and clay. The biogenic Mn and Fe record the passage of time, whereas the accumulation of clay particles is a more time-random process. X-ray fluorescence (XRF) can measure just the "metal thickness" of Mn and Fe in varnish. Earlier tedious microscope techniques focused on physical thickness that includes the noise associated with the clay component. XRF integrates the metal thickness of a broad area of varnish, which is seen to vary significantly in a thin-section traverse. Thus XRF provides a meaningful average thickness over a surface. A portable x-ray fluorescence unit provides rapid, non-destructive, in situ measurements. On outcrop a single analysis takes about 2 minutes and the varnish is not consumed or even disturbed. The hand-held PXRF instrument is simple to operate and relatively inexpensive (\\$ 30,000). PXRF analysis of varnish on independently dated materials yielded a substantive correlation between age and metal (Mn + Fe) thickness. This provided an initial validation of the

  6. Analysis Results for Lunar Soil Simulant Using a Portable X-Ray Fluorescence Analyzer

    NASA Technical Reports Server (NTRS)

    Boothe, R. E.

    2006-01-01

    Lunar soil will potentially be used for oxygen generation, water generation, and as filler for building blocks during habitation missions on the Moon. NASA s in situ fabrication and repair program is evaluating portable technologies that can assess the chemistry of lunar soil and lunar soil simulants. This Technical Memorandum summarizes the results of the JSC 1 lunar soil simulant analysis using the TRACeR III IV handheld x-ray fluorescence analyzer, manufactured by KeyMaster Technologies, Inc. The focus of the evaluation was to determine how well the current instrument configuration would detect and quantify the components of JSC-1.

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

    NASA Astrophysics Data System (ADS)

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

    1999-12-01

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

  8. Combined backscatter Moessbauer spectrometer/x ray fluorescence analyzer (BaMS/XRF) for extraterrestrial surfaces

    NASA Technical Reports Server (NTRS)

    Shelfer, T. D.; Wills, E. L.; Agresti, D. G.; Pimperl, M. M.; Shen, M. H.; Morris, R. V.; Nguyen, T.

    1993-01-01

    We have designed and tested a prototype combined backscatter Moessbauer spectrometer and x-ray fluorescence analyzer (BaMS/XRF). A space qualified instrument based on this design would be suitable for in-situ use on planetary missions to the surfaces of the Moon (Artemis and lunar outpost), Mars (MESUR), asteroids, or other solid solar system objects. The BaMS/XRF instrument is designed to be capable of concurrent sample analyses for the mineralogy of iron-bearing phases and elemental composition without the need for sample preparation.

  9. In-vivo Fluorescent X-ray CT Imaging of Mouse Brain

    SciTech Connect

    Takeda, T.; Wu, J.; Lwin, Thet-Thet; Huo, Q.; Minami, M.; Sunaguchi, N.; Murakami, T.; Mouri, S.; Nasukawa, S.; Yuasa, T.; Akatsuka, T.; Hyodo, K.; Hontani, H.

    2007-01-19

    Using a non-radioactive iodine-127 labeled cerebral perfusion agent (I-127 IMP), fluorescent X-ray computed tomography (FXCT) clearly revealed the cross-sectional distribution of I-127 IMP in normal mouse brain in-vivo. Cerebral perfusion of cortex and basal ganglion was depicted with 1 mm in-plane spatial resolution and 0.1 mm slice thickness. Degree of cerebral perfusion in basal ganglion was about 2-fold higher than that in cortical regions. This result suggests that in-vivo cerebral perfusion imaging is realized quantitatively by FXCT at high volumetric resolution.

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

    USGS Publications Warehouse

    Beyermann, K.; Rose, H.J., Jr.; Christian, R.P.

    1969-01-01

    Nanogram amounts of chromium can be extracted as oxinate into chloform. By treatment of the chloroform layer 3 M hydrochloric acid, oxinates of other elements and excess of reagent are removed, leaving a chloroform solution of the chromium chelate only. This solution is concentrated and transferred to the top of a small brass rod acting as sample holder. The intensity of the X-ray fluorescence of the Cr K?? line is measured with curved crystal optics. Chromium amounts greater than 5 ng can be detected. The application of the procedure to the analysis of the chromium content of urine is demonstrated. ?? 1969.

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

    SciTech Connect

    Covert, Timothy Todd

    2014-09-01

    The Light Initiated High Explosive facility utilized a spray deposited coating of silver acetylide - silver nitrate explosive to impart a mechanical shock into targets of interest. A diagnostic was required to measure the explosive deposition in - situ. An X - ray fluorescence spectrometer was deployed at the facility. A measurement methodology was developed to measure the explosive quantity with sufficient accuracy. Through the use of a tin reference material under the silver based explosive, a field calibration relationship has been developed with a standard deviation of 3.2 % . The effect of the inserted tin material into the experiment configuration has been explored.

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

    SciTech Connect

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

    2014-04-24

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

  13. X-ray fluorescence in investigations of cultural relics and archaeological finds.

    PubMed

    Musílek, Ladislav; Cechák, Tomáš; Trojek, Tomáš

    2012-07-01

    Some characteristic features of X-ray fluorescence (XRF) analysis make it an ideal method for investigations of cultural relics and archaeological finds. It has therefore become a standard method used in archaeometry. Paintings, frescos, manuscripts, pottery, metalwork, glass, and many other objects are analysed with the aim of recognising their materials, production technologies and origin, and for identifying counterfeits. This paper reviews various techniques used in XRF analyses of works of art, summarises the advantages and limitations of the method, and presents some typical examples of its use. The general review is supplemented by some techniques used and some results achieved at CTU-FNSPE in Prague. PMID:22099447

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

    NASA Astrophysics Data System (ADS)

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

    2013-10-01

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

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

    NASA Astrophysics Data System (ADS)

    Ayala Jiménez, Rony E.

    2001-11-01

    Multielement analysis by total reflection X-ray fluorescence spectrometry has evolved during two decades. At present commercial equipment is available for chemical analysis of all types of biological and mineral samples. The electronic industry has also benefited from scientific and technological developments in this field due to new instrumentation to determine contamination on the surface of silicon wafers (the equipment will not be covered in this paper). The basic components of the spectrometers can be summarized as follows: (a) excitation source; (b) geometric arrangement (optics) for collimation and monochromatization of the primary radiation; (c) X-ray detector; and (d) software for operation of the instrument, data acquisition and spectral deconvolution to determine the concentrations of the elements (quantitative analysis). As an optional feature one manufacturer offers a conventional 45° geometry for direct excitation. Personal communications of the author and commercial brochures available have allowed us to list the components used in TXRF for multielement analysis. Excitation source: high-power sealed X-ray tubes, output from 1300 to 3000 W, different mixed alloy anodes Mo/W are used but molybdenum, tungsten and copper are common; single anode metal ceramic low power X-ray tubes, output up to 40 W. Excitation systems can be customized according to the requirements of the laboratory. Detector: silicon-lithium drifted semiconductor detector liquid nitrogen cooled; or silicon solid state thermoelectrically cooled detector (silicon drift detector SDD and silicon-PIN diode detector). Optics: multilayer monochromator of silicon-tungsten, nickel-carbon or double multilayer monochromator. Electronics: spectroscopy amplifier, analog to digital converter adapted to a PC compatible computer with software in a Windows environment for the whole operation of the spectrometer and for qualitative/quantitative analysis of samples are standard features in the

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

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Van Pevenage, Jolien; De Langhe, Kaat; De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo; Vandenabeele, Peter; Martens, Maximiliaan P. J.

    2014-07-01

    "Mad Meg", a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO2 + 15% K2O + 10% CoO + 5% Al2O3) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel.

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

    NASA Astrophysics Data System (ADS)

    Manso, M.; Valadas, S.; Pessanha, S.; Guilherme, A.; Queralt, I.; Candeias, A. E.; Carvalho, M. L.

    2010-04-01

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

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

    SciTech Connect

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

    2008-01-15

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

  20. New results in high-resolution X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Žitnik, Matjaž; Kavčič, Matjaž; Bučar, Klemen; Mihelič, Andrej; Bohinc, Rok

    2014-04-01

    We present some recent results dealing with resonant inelastic X-ray scattering (RIXS) on atomic targets in the 3-5 keV enegy region. In this so-called tender spectral region, the K-shell fluorescence branching ratios become reasonably large, but a full vacuum enclosure is still preferable to avoid detection efficiency loss due to the sizeable arms of high resolution crystal spectrometers. By squeezing energy resolution in the fluorescence decay channel, one may improve the spectral resolution of photoabsorption, enable separation of multielectron excitation and relaxation channels, and completely eliminate the need to scan across the selected energy range of the photon probe in order to acquire the photoabsorption spectrum. On the other hand, the spectra may be untrivially modified by effects such as interference of absorption-emission paths or structured relaxation modes, and a more elaborated modelling is needed to understand the emitted signal. We illustrate these aspects by presenting four cases: the reconstruction of Ar KM and Ar KL absorption edges from a series of highly resolved emission spectra recorded at different probe energies, the reconstruction of the Xe L3 edge from a single X-ray emission spectrum, and the analysis of the radiative Ar K-MM Auger decay preceeded by the resonant or nonresonant photon absorption.

  1. A robust X-ray fluorescence technique for multielemental analysis of solid samples.

    PubMed

    Kallithrakas-Kontos, Nikolaos; Foteinis, Spyros; Paigniotaki, Katherine; Papadogiannakis, Minos

    2016-02-01

    X-ray fluorescence (XRF) quantitation software programs are widely used for analyzing environmental samples due to their versatility but at the expense of accuracy. In this work, we propose an accurate, robust, and versatile technique for multielemental X-ray fluorescence analytical applications, by spiking solid matrices with standard solutions. National Institute of Standards and Technology (NIST)-certified soil standards were spiked with standard solutions, mixed well, desiccated, and analyzed by an energy dispersive XRF. Homogenous targets were produced and low error calibration curves, for the added and not added, neighboring, elements, were obtained. With the addition of few elements, the technique provides reliable multielemental analysis, even for concentrations of the order of milligram per kilogram (ppm). When results were compared to the ones obtained from XRF commercial quantitation software programs, which are widely used in environmental monitoring and assessment applications, they were found to fit certified values better. Moreover, in all examined cases, results were reliable. Hence, this technique can also be used to overcome difficulties associated with interlaboratory consistency and for cross-validating results. The technique was applied to samples with an environmental interest, collected from a ship/boat repainting area. Increased copper, zinc, and lead loads were observed (284, 270, and 688 mg/kg maximum concentrations in soil, respectively), due to vessels being paint stripped and repainted. PMID:26815558

  2. Analytical approaches for determination of bromine in sediment core samples by X-ray fluorescence spectrometry.

    PubMed

    Pashkova, Galina V; Aisueva, Tatyana S; Finkelshtein, Alexander L; Ivanov, Egor V; Shchetnikov, Alexander A

    2016-11-01

    Bromine has been recognized as a valuable indicator for paleoclimatic studies. Wavelength dispersive X-ray fluorescence (WDXRF) and total reflection X-ray fluorescence (TXRF) methods were applied to study the bromine distributions in lake sediment cores. Conventional WDXRF technique usually requires relatively large mass of a sediment sample and a set of calibration samples. Some analytical approaches were developed to apply WDXRF to small sediment core samples in the absence of adequate calibration samples with a known Br content. The mass of a sample to be analyzed was reduced up to 200-300mg and the internal standard method with correction using fundamental parameters was developed for Br quantification. TXRF technique based on the direct analysis of a solid suspension using 20mg of sediment sample by internal standard method was additionally tested. The accuracy of the WDXRF and TXRF techniques was assessed by the comparative analysis of reference materials of sediments, soil and biological samples. In general, good agreement was achieved between the reference values and the measured values. The detection limits of Br were 1mg/kg and 0.4mg/kg for WDXRF and TXRF respectively. The results of the Br determination obtained with different XRF techniques were comparable to each other and used for paleoclimatic reconstructions. PMID:27591627

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

    SciTech Connect

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

    2008-01-01

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

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

    PubMed

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

    2013-01-01

    This work presents a study of human hair as a bio-indicator for detection of heavy metals as part of environmental health surveillance programs project to develop a subject of interest in the biomedical and environmental sciences. A total of 34 hair samples were analyzed that consisting of 29 samples from sanitation workers and five samples from students. The hair samples were prepared and treated in accordance to the International Atomic Energy Agency (IAEA) recommendations. The concentrations of heavy metals were analyzed using the energy dispersive X-ray fluorescence (EDXRF) technique by X-50 Mobile X-ray Fluorescence (XRF) at Oceanography Institute, Universiti Malaysia Terengganu. The performance of EDXRF analyzer was tested by Standard Reference Material (SRM 2711) Montana Soil which was in good agreement with certified value within 14% deviations except for Hg. While seven heavy metals: Mn, Fe, Ni, Cu, Zn, Se, and Sb were detected in both groups, three additional elements, i.e. As, Hg and Pb, were detected only in sanitation workers group. For sanitation workers group, the mean concentration of six elements, Mn, Fe, Cu, Zn, Se, and Sb, shows elevated concentration as compared to the control samples concentration. Results from both groups were compared and discussed in relation to their respective heavy metals concentrations. PMID:22846873

  5. Determination of selenium in biological samples with an energy-dispersive X-ray fluorescence spectrometer.

    PubMed

    Li, Xiaoli; Yu, Zhaoshui

    2016-05-01

    Selenium is both a nutrient and a toxin. Selenium-especially organic selenium-is a core component of human nutrition. Thus, it is very important to measure selenium in biological samples. The limited sensitivity of conventional XRF hampers its widespread use in biological samples. Here, we describe the use of high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-Ray fluorescence spectroscopy (EDXRF) in tandem with a three-dimensional optics design to determine 0.1-5.1μgg(-1) levels of selenium in biological samples. The effects of various experimental parameters such as applied voltage, acquisition time, secondary target and various filters were thoroughly investigated. The detection limit of selenium in biological samples via high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-ray fluorescence spectroscopy was decreased by one order of magnitude versus conventional XRF (Paltridge et al., 2012) and found to be 0.1μg/g. To the best of our knowledge, this is the first report to describe EDXRF measurements of Se in biological samples with important implications for the nutrition and analytical chemistry communities. PMID:26922394

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  7. Study of gold nanoparticle synthesis by synchrotron x-ray diffraction and fluorescence

    NASA Astrophysics Data System (ADS)

    Yan, Zhongying; Wang, Xiao; Yu, Le; Moeendarbari, Sina; Hao, Yaowu; Cai, Zhonghou; Cheng, Xuemei

    Gold nanoparticles have a wide range of potential applications, including therapeutic agent delivery, catalysis, and electronics. Recently a new process of hollow nanoparticle synthesis was reported, the mechanism of which was hypothesized to involve electroless deposition around electrochemically evolved hydrogen bubbles. However, the growth mechanism still needs experimental evidence. We report investigation of this synthesis process using synchrotron x-ray diffraction and fluorescence measurements performed at beamline 2-ID-D of the Advanced Photon Source (APS). A series of gold nanoparticle samples with different synthesis time (50-1200 seconds) were deposited using a mixture electrolyte solution of Na3Au(SO3)2 and H4N2NiO6S2 on anodic aluminum oxide (AAO) membranes. The 2D mapping of fluorescence intensity and comparison of x-ray diffraction peaks of the samples have provided valuable information on the growth mechanism. Work at Bryn Mawr College and University of Texas at Arlington is supported by NSF Grants (1207085 and 1207377) and use of the APS at Argonne National Laboratory is supported by the U. S. Department of Energy under Contract No. DE-AC02-06CH11357.

  8. Use of x-ray fluorescence for in-situ detection of metals

    NASA Astrophysics Data System (ADS)

    Elam, W. T. E.; Whitlock, Robert R.; Gilfrich, John V.

    1995-01-01

    X-ray fluorescence (XRF) is a well-established, non-destructive method of determining elemental concentrations at ppm levels in complex samples. It can operate in atmosphere with no sample preparation, and provides accuracies of 1% or better under optimum conditions. This report addresses two sets of issues concerning the use of x-ray fluorescence as a sensor technology for the cone penetrometer, for shipboard waste disposal, or for other in-situ, real- time environmental applications. The first issue concerns the applicability of XRF to these applications, and includes investigation of detection limits and matrix effects. We have evaluated the detection limits and quantitative accuracy of a sensor mock-up for metals in soils under conditions expected in the field. In addition, several novel ways of improving the lower limits of detection to reach the drinking water regulatory limits have been explored. The second issue is the engineering involved with constructing a spectrometer within the 1.75 inch diameter of the penetrometer pipe, which is the most rigorous physical constraint. Only small improvements over current state-of-the-art are required. Additional advantages of XRF are that no radioactive sources or hazardous materials are used in the sensor design, and no reagents or any possible sources of ignition are involved.

  9. The BioCAT Microprobe for X-Ray Fluorescence Imaging, MicroXAFS and Microdiffraction Studies on Biological Samples

    SciTech Connect

    Barrea, R.A.; Gore, D.; Kondrashkina, E.; Weng, T.; Heurich, R.; Vukonich, M.; Orgel, J.; Davidson, M.; Collingwood, J.F.; Mikhaylova, A.; Irving, T.C.

    2007-07-31

    Microbeam capabilities have been recently added to the Biophysics Collaborative Access Team (BioCAT) beamline 18-ID at the Advanced Photon Source to allow x-ray elemental mapping, micro x-ray absorption fine structure and microdiffraction studies on biological samples. The microprobe setup comprises a pair of platinum coated silicon KB mirrors; a sample holder mounted in a high precision positioner (100 nm accuracy); fluorescence detectors including a Si drift detector, Fe and Zn Bent Laue analyzers and a Ge detector; and a CCD detector for micro-diffraction experiments. The energy range of the microprobe is from 3.5 keV up to 17 keV. The fast scanning capabilities of the Bio-CAT beamline facilitate rapid acquisition of x-ray elemental images and micro-XAFS spectra. This paper reports the results of commissioning the KB mirror system and its performance in initial x-ray fluorescence mapping and micro-diffraction studies.

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

    NASA Astrophysics Data System (ADS)

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

    2012-09-01

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

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

    PubMed

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

    2014-09-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

  13. Direct spectral recovery using X-ray fluorescence measurements for material decomposition applications using photon counting spectral X-ray detectors

    NASA Astrophysics Data System (ADS)

    Campbell-Ricketts, Tom; Das, Mini

    2014-03-01

    We present investigations into direct, calibration-free recovery of distorted spectral x-ray measurements with the Medipix 2 detector. Spectral x-ray measurements using pixelated photon counting spectral x-ray detectors are subject to significant spectral distortion. For detectors with small pixel size, charge sharing between adjacent electrodes often dominates this distortion. In material decomposition applications, a popular spectral recovery technique employs a calibration phantom with known spectral properties. This works due to the similarity of the attenuation properties of the phantom and the material to be studied. However, this approach may be too simplistic for clinical imaging applications as it assumes the homogeneity (and knowledge) of exactly the properties whose variation accounts entirely for the diagnostic content of the spectral data obtained by the photon counting detector. It may also be difficult to find the right calibration phantom for varying patient size and tissue densities on a case-by-case basis. Thus, it is desirable to develop direct correction strategies, based on the objectively measurable response of the detector. We model analytically the distortion of a spectral signal in a PCSXD by applying Gaussian broadening and a charge-sharing model. The model parameters are fitted to the measured fluorescence of several metals. While we are investigating the methodology using Medipix detectors, it should be applicable to other PCXDs as well.

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

    NASA Technical Reports Server (NTRS)

    Kelliher, Warren C.; Partos, Richard D.; Nelson, Irina

    1996-01-01

    The objective of this project was to assess the sensitivity of X-ray Fluorescence Spectroscopy (XFS) for quantitative evaluation of metal particle content in engine oil suspensions and the feasibility of real-time, dynamic wear metal analysis. The study was focused on iron as the majority wear metal component. Variable parameters were: particle size, particle concentration and oil velocity. A commercial XFS spectrometer equipped with interchangeable static/dynamic (flow cell) sample chambers was used. XFS spectra were recorded for solutions of Fe-organometallic standard and for a series of DTE oil suspensions of high purity spherical iron particles of 2g, 4g, and 8g diameter, at concentrations from 5 ppm to 5,000 ppm. Real contaminated oil samples from Langley Air Force Base aircraft engines and NASA Langley Research Center wind tunnels were also analyzed. The experimental data conform the reliability of XFS as the analytical method of choice for this project. Intrinsic inadequacies of the instrument for precise analytic work at low metal concentrations were identified as being related to the particular x-ray beam definition, system geometry, and flow-cell materials selection. This work supports a proposal for the design, construction and testing of a conceptually new, miniature XFS spectrometer with superior performance, dedicated to on-line, real-time monitoring of lubricating oils in operating engines. Innovative design solutions include focalization of the incident x-ray beam, non-metal sample chamber, and miniaturization of the overall assembly. The instrument would contribute to prevention of catastrophic engine failures. A proposal for two-year funding has been presented to NASA Langley Research Center Internal Operation Group (IOG) Management, to continue the effort begun by this summer's project.

  15. Measuring lead, mercury, and uranium by in vivo X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    O'Meara, Joanne Michelle

    X-ray fluorescence (XRF) has been demonstrated to be a useful technique for measuring trace quantities of heavy metals in various tissues within the body. This thesis investigates a means of improving the measurement of lead in bone, as well as increasing the existing sensitivity of measuring kidney mercury content. The XRF measurement of uranium is also explored. This work assesses the feasibility of a normalisation method for the 57Co/90° system, in relating detected signal to the lead content of the sample. The feasibility of normalisation has been shown, which reduces subject dose and improves system transportability, as well as removes subjectivity, by eliminating the need for acquiring planar x-ray images of the measurement site. In the measurement of renal mercury concentrations, a gain in sensitivity increasing the x-ray tube operating voltage of the current system is investigated. It found that 250 kV, rather than 175 kV, and a titanium rather than uranium filter, results in a 2.5 +/- 0.2 times gain in sensitivity. This potential improvement could have profound clinical implications for the accuracy of occupational monitoring, and for assessing whether there is a quantitative relationship between biological fluid levels and mercury content in this critical organ. The XRF measurement of bone uranium content is also explored. Both source-excited and polarised systems have been developed, however, the sensitivity is currently beyond that which is useful for occupational monitoring of exposure to this toxin. The particular case of measuring uranium in survivors of "Friendly Fire" incidents (from Operation Desert Storm) is investigated, and the first detectable quantity of uranium has been observed in a member of this cohort, with the XRF system designed and built during the course of this work.

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

    SciTech Connect

    Lawniczak-Jablonska, K. |; Jia, J.J.; Underwood, J.H.

    1997-04-01

    As modern, technologically important materials have become more complex, element specific techniques have become invaluable in studying the electronic structure of individual components from the system. Soft x-ray fluorescence (SXF) and absorption (SXA) spectroscopies provide a unique means of measuring element and angular momentum density of electron states, respectively, for the valence and conducting bands in complex materials. X-ray absorption and the decay through x-ray emission are generally assumed to be two independent one-photon processes. Recent studies, however have demonstrated that SXF excited near the absorption threshold generate an array of spectral features that depend on nature of materials, particularly on the localization of excited states in s and d-band solids and that these two processes can no be longer treated as independent. Resonant SXF offers thus the new way to study the dynamics of the distribution of electronic valence states in the presence of a hole which is bound to the electron low lying in the conduction band. This process can simulate the interaction between hole-electron pair in wide gap semiconductors. Therefore such studies can help in understanding of transport and optics phenomena in the wide gap semiconductors. The authors report the result of Mn and S L-resonant emission in Zn{sub 1{minus}x}Mn{sub x}S (with x=0.2 and 0.3) and MnS as the energy of exciting radiation is tuned across the Mn and S L{sub 3,2} absorption edge, along with the resonant excited spectra from elemental Mn as a reference.

  17. Micro energy dispersive X-ray fluorescence analysis of polychrome lead-glazed Portuguese faiences

    NASA Astrophysics Data System (ADS)

    Guilherme, A.; Pessanha, S.; Carvalho, M. L.; dos Santos, J. M. F.; Coroado, J.

    2010-04-01

    Several glazed ceramic pieces, originally produced in Coimbra (Portugal), were submitted to elemental analysis, having as premise the pigment manufacture production recognition. Although having been produced in Coimbra, their location changed as time passed due to historical reasons. A recent exhibition in Coimbra brought together a great number of these pieces and in situ micro Energy Dispersive X-ray Fluorescence (µ-EDXRF) analyses were performed in order to achieve some chemical and physical data on the manufacture of faiences in Coimbra. A non-commercial µ-EDXRF equipment for in situ analysis was employed in this work, carrying some important improvements when compared to the conventional ones, namely, analyzing spot sizes of about 100 µm diameter. The combination of a capillary X-ray lens with a new generation of low power microfocus X-ray tube and a drift chamber detector enabled a portable unit for micro-XRF with a few tens of µm lateral resolution. The advantages in using a portable system emphasized with polycapillary optics enabled to distinguish proximal different pigmented areas, as well as the glaze itself. These first scientific results on the pigment analysis of the collection of faiences seem to point to a unique production center with own techniques and raw materials. This conclusion arose with identification of the blue pigments having in its constitution Mn, Fe Co and As and the yellows as a result of the combination between Pb and Sb. A statistical treatment was used to reveal groups of similarities on the pigments elemental profile.

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

    SciTech Connect

    Worley, C. G.; Wiltshire, S.; Miller, T. C.; Havrilla, G. J.; Majidi, V.

    2005-01-01

    A method was developed to detect fingerprints using a technique known as micro-X-ray fluorescence. The traditional method of detecting fingerprints involves treating the sample with certain powders, liquids, or vapors to add color to the fingerprint so that it can be easily seen and photographed for forensic purposes. This is known as contrast enhancement, and a multitude of chemical processing methods have been developed in the past century to render fingerprints visible. However, fingerprints present on certain substances such as fibrous papers and textiles, wood, leather, plastic, adhesives, and human skin can sometimes be difficult to detect by contrast enhancement. Children's fingerprints are also difficult to detect due to the absence of sebum on their skin, and detection of prints left on certain colored backgrounds can sometimes be problematic. Micro-X-ray fluorescence (MXRF) was studied here as a method to detect fingerprints based on chemical elements present in fingerprint residue. For example, salts such as sodium chloride and potassium chloride excreted in sweat are sometimes present in detectable quantities in fingerprints. We demonstrated that MXRF can be used to detect this sodium, potassium, and chlorine from such salts. Furthermore, using MXRF, each of these elements (and many other elements if present) can be detected as a function of location on a surface, so we were able to 'see' a fingerprint because these salts are deposited mainly along the patterns present in a fingerprint (traditionally called friction ridges in forensic science). MXRF is not a panacea for detecting all fingerprints; some prints will not contain enough detectable material to be 'seen'; however, determining an effective means of coloring a fingerprint with traditional contrast enhancement methods can sometimes be an arduous process with limited success. Thus, MXRF offers a possible alternative for detecting fingerprints, and it does not require any additional chemical

  19. Genesis Sample Surface Contamination Study using Total-reflection X-Ray Fluorescence (TXRF)

    NASA Astrophysics Data System (ADS)

    Brennan, S.; Luening, K.; Pianetta, P.; Ishii, H. A.; Burnett, D. S.

    2005-12-01

    We have used synchrotron-based Total-reflection X-Ray Fluorescence (TXRF) to measure the surface and near-surface contamination of Genesis flight spare material as well as one piece of sapphire which flew on the mission. Flight spare samples included uncoated, Al-coated and Au-coated sapphire wafers and diamond-like carbon (DLC) on silicon. These studies were performed to determine the suitability of TXRF for the study of Genesis materials. The technique is optimally suited and highly surface sensitive for elements between Na and Br with sensitivities ranging from 1e9 to 1e12 atoms/cm2. By changing the x-ray angle of incidence one can vary the sampling depth from ~ 100 Å to several thousand Å. We found that the level of contamination of the flight-spare material varied widely. For the case of the returned piece of sapphire there were concentrations of Ge on the surface approaching monolayer coverage.

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

    SciTech Connect

    Bucher, J.J.; Allen, P.G.; Edelstein, N.M.; Shuh, D.K.; Madden, N.W.; Cork, C.; Luke, P.; Pehl, D.; Malone, D.

    1995-03-01

    Construction and performance of a monolithic quad-pixel Ge detector for fluorescence x-ray absorption spectroscopy (XAS) at synchrotron radiation sources are described. The detector semiconductor element has an active surface area of 4.0 cm{sup 2} which is electrically separated into four 1.0 cm{sup 2} pixels, with little interfacial dead volume. Spatial response of the array shows that cross-talk between adjacent pixels is < 10% for 5.9 keV photons that fall within 0.5 mm of the pixel boundaries. The detector electronics system uses pre-amplifiers built at LBNL with commercial Tennelec Model TC 244 amplifiers. Using an {sup 55}Fe test source (MnK{sub {alpha}}, 5.9 keV), energy resolution of better than 200 eV is achieved with a 4 {mu}sec peaking time. At 0.5 {mu}sec peaking time, pulse pileup results in a 75% throughput efficiency for an incoming count rate of 100 kHz. Initial XAS fluoresncece measurements at the beamline 4 wiggler end stations at SSRL show that the detector system has several advantages over commercial x-ray spectrometers for low-concentration counting.

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

    PubMed

    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. PMID:23561904

  2. Lunar X-ray fluorescence spectrometery with the Selene orbiter: science and instrument

    NASA Astrophysics Data System (ADS)

    Okada, T.; Shirai, K.; Yamamoto, Y.; Arai, T.; Ogawa, K.; Kato, M.; Selene Xrs Team

    We have been developing an X-ray fluorescence spectrometer, XRS, for the SELENE lunar orbiter mission to map major elemental composition of the Moon as well as to understand the mechanism of X-ray excitation in the nightside and physical properties caused by surface materials. We present here scientific objectives and instrumentation of the XRS, since a critical design review and satellite interface test has been finished and the flight model is now in preparation. The XRS is based on charge-coupled devices with heritage technology after the S310-28 sounding rocket experiment in 1999 and HAYABUSA (former MUSES-C) asteroid mission launched in 2003 but has been redesigned most suitable for lunar mission and improved its performance. The detection area of 100cm2 and FOV of 12 deg enables to limit the footprint of 20km. Utilization of CCD under more stable control of temperature and short integration time increases the apparent energy resolution. On the SELENE around the lunar polar orbit, total surface coverage except for the polar region will be achieved. The mission is now in the component calibration phase after satellite interface tests has been finished. The XRS is in final preparation for flight and has been also examined in detail its function and performance in the laboratory.

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

    SciTech Connect

    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.

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

    SciTech Connect

    Rajasingam, Akshayan; Hoover, Andrew S; Fensin, Michael L; Tobin, Stephen J

    2009-01-01

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

  5. Total reflection X-ray fluorescence (TXRF) for direct analysis of aerosol particle samples.

    PubMed

    Bontempi, E; Zacco, A; Benedetti, D; Borgese, L; Colombi, P; Stosnach, H; Finzi, G; Apostoli, P; Buttini, P; Depero, L E

    2010-04-14

    Atmospheric aerosol particles have a great impact on the environment and on human health. Routine analysis of the particles usually involves only the mass determination. However, chemical composition and phases provide fundamental information about the particles' origins and can help to prevent health risks. For example, these particles may contain heavy metals such as Pb, Ni and Cd, which can adversely affect human health. In this work, filter samples were collected in Brescia, an industrial town located in Northern Italy. In order to identify the chemical composition and the phases of the atmospheric aerosols, the samples were analysed by means of total reflection X-ray fluorescence (TXRF) spectrometry with a laboratory instrument and X-ray microdiffraction at Synchrotron Daresbury Laboratories, Warrington (Cheshire, UK). The results are discussed and correlated to identify possible pollution sources. The novelty of this analytical approach is that filter samples for TXRF were analysed directly and did not require chemical pretreatment to leach elements from the aerosol particulates. The results of this study clearly show that TXRF is a powerful technique for the analysis of atmospheric aerosols on 'as-received' filters, thereby leaving samples intact and unaltered for possible subsequent analyses by other methods. In addition, the low detection limits for many elements (low ng/cm2) indicate that this method may hold promise in various application fields, such as nanotechnology. PMID:20480822

  6. Analysis of Russian kopecks (1877-1933) using x-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Cavness, B.; Williams, S.

    2013-04-01

    We have analyzed five Russian kopecks minted between the years of 1877 and 1933 using X-ray fluorescence (XRF) as part of an undergraduate research project. The intensities of the Cu K-shell X-rays were studied in order to compare the relative purities of the Cu used to mint the kopecks. The economic conditions under which the kopecks were minted are discussed, as well as impurities discovered during XRF analysis. In addition to XRF analysis, kopecks produced just before (1915) and after (1924) the October Revolution of 1917 were weighed in order to determine whether or not the Decree of February 22, 1924 was carried out. The legislation (enacted by the Central Executive Committee and the Council of the People's Commissaries) decreed that the proportions of pure Ag and Cu used in the minting of new coins should be the identical to those produced before the revolution and that the diameters and weights of the kopecks should also remain the same. The data from our experiments suggest that the legislation was successfully carried out.

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

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

  8. Lithographically-fabricated channel arrays for confocal x-ray fluorescence microscopy and XAFS

    NASA Astrophysics Data System (ADS)

    Woll, Arthur R.; Agyeman-Budu, David; Choudhury, Sanjukta; Coulthard, Ian; Finnefrock, Adam C.; Gordon, Robert; Hallin, Emil; Mass, Jennifer

    2014-03-01

    Confocal X-ray Fluorescence Microscopy (CXRF) employs overlapping focal regions of two x-ray optics—a condenser and collector—to directly probe a 3D volume. The minimum-achievable size of this probe volume is limited by the collector, for which polycapillaries are generally the optic of choice. Recently, we demonstrated an alternative collection optic for CXRF, consisting of an array of micron-scale collimating channels, etched in silicon, and arranged like spokes of a wheel directed towards a single source position. The optic, while successful, had a working distance of only 0.2 mm and exhibited relatively low total collection efficiency, limiting its practical application. Here, we describe a new design in which the collimating channels are formed by a staggered array of pillars whose side-walls taper away from the channel axis. This approach improves both collection efficiency and working distance, while maintaining excellent spatial resolution. We illustrate these improvements with confocal XRF data obtained at the Cornell High Energy Synchrotron Source (CHESS) and the Advanced Photon Source (APS) beamline 20-ID-B.

  9. In vivo monitoring of toxic metals: assessment of neutron activation and x-ray fluorescence techniques

    SciTech Connect

    Ellis, K.J.

    1986-01-01

    To date, cadmium, lead, aluminum, and mercury have been measured in vivo in humans. The possibilities of monitoring other toxic metals have also been demonstrated, but no human studies have been performed. Neutron activation analysis appears to be most suitable for Cd and Al measurements, while x-ray fluorescence is ideally suited for measurement of lead in superficial bone. Filtered neutron beams and polarized x-ray sources are being developed which will improve in vivo detection limits. Even so, several of the current facilities are already suitable for use in epidemiological studies of selected populations with suspected long-term low-level ''environmental'' exposures. Evaluation and diagnosis of patients presenting with general clinical symptoms attributable to possible toxic metal exposure may be assisted by in vivo examination. Continued in vivo monitoring of industrial workers, especially follow-up measurements, will provide the first direct assessment of changes in body burden and a direct measure of the biological life-times of these metals in humans. 50 refs., 4 figs., 2 tabs.

  10. Synchrotron radiation induced μ-X-ray fluorescence spectroscopy on municipal solid waste fly ashes

    NASA Astrophysics Data System (ADS)

    Camerani, Maria Caterina; Somogyi, Andrea; Drakopoulos, Mikael; Steenari, Britt-Marie

    2001-08-01

    The high brightness of synchrotron radiation sources of the 3rd generation and the development of focusing optical elements for X-rays make it possible to create beams of micrometer size with high intensity. These beams can be used to reveal spatially resolved information about structural and chemical properties of particles. Here, the possibility of using synchrotron radiation micro-X-ray fluorescence (μ-SRXRF) for the determination of the major and minor components and their distribution within municipal solid waste (MSW) fly ashes has been investigated. By using an excitation energy of 27.0 keV, trace elements of environmental concern, like Cd, Pb and Zn can be detected to their low concentrations (ppm) routinely. The aim of the work was to gain a better understanding of the factors that determine the environmental mobility of each trace element and, in particular, the potential for their dissolution and leaching. Such detailed investigation of the content and distribution of toxic metals on/in individual particles is a valuable complement to the usual elemental analysis of bulk samples.

  11. Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

    PubMed

    Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

    2016-03-15

    A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles. PMID:26891032

  12. Imaging metals in proteins by combining electrophoresis with rapid x-ray fluorescence mapping.

    SciTech Connect

    Finney, L.; Chishti, Y.; Khare, T.; Giometti, C.; Levina, A.; Lay, P. A.; Vogt, S.; Univ. of Sydney; Northwestern Univ.

    2010-01-01

    Growing evidence points toward a very dynamic role for metals in biology. This suggests that physiological circumstance may mandate metal ion redistribution among ligands. This work addresses a critical need for technology that detects, identifies, and measures the metal-containing components of complex biological matrixes. We describe a direct, user-friendly approach for identifying and quantifying metal?protein adducts in complex samples using native- or SDS-PAGE, blotting, and rapid synchrotron X-ray fluorescence mapping with micro-XANES (X-ray absorption near-edge structure) of entire blots. The identification and quantification of each metal bound to a protein spot has been demonstrated, and the technique has been applied in two exemplary cases. In the first, the speciation of the in vitro binding of exogenous chromium to blood serum proteins was influenced markedly by both the oxidation state of chromium exposed to the serum proteins and the treatment conditions, which is of relevance to the biochemistry of Cr dietary supplements. In the second case, in vivo changes in endogenous metal speciation were examined to probe the influence of oxygen depletion on iron speciation in Shewanella oneidensis.

  13. Micro x-ray fluorescence as a high throughput screening method for metal chelating compounds

    NASA Astrophysics Data System (ADS)

    Minogue, Edel M.; Havrilla, George J.; Taylor, Tammy P.; Burrell, Anthony K.; Warner, Benjamin P.

    2005-06-01

    Micro X-ray Fluorescence (MXRF) has proven to be a powerful tool in the rapid and quantitative means of screening oliogpeptides. MXRF is a non-destructive method of analysis, which can detect elemental composition of a sample by measuring its characteristic X-ray emission wavelengths or energies. An effective high throughput screening technique is described for the rapid screening of bead-based libraries by MXRF in order to identify suitable chelating agents that will bind metals found in radioactive dispersive devices. It is a sensitive technique which in conjunction with the wide range of chemistry inherent in peptide libraries (e.g. varying charge, length, hydrophobicity, aromaticity etc.), provides a rapid and quantitative means for screening chelator-ion binding. The method involves the selection of a suitable library of ligands; in this case it is a bead-based library of peptides. The library is exposed to the cation of interest and immobilized on to a microarray. The array is then analyzed by MXRF enabling rapid identification of chelating agents. This enables the screening of approximately 27,500 sequences per day. Initial experiments carried out successfully identified sequences that are selective for Co under certain binding conditions. This involved the screening of 8,400 sequences in adverse environmental conditions containing possible interferences (e.g. Ca, Fe, Al, Cs, Ir), which could be encountered in our application.

  14. Brain Iron Detected by SWI High Pass Filtered Phase Calibrated with Synchrotron X-Ray Fluorescence

    PubMed Central

    Hopp, Karla; Popescu, Bogdan F.Gh.; McCrea, Richard P.E.; Harder, Sheri L.; Robinson, Christopher A.; Haacke, Mark E.; Rajput, Ali H.; Rajput, Alex; Nichol, Helen

    2013-01-01

    Purpose To test the ability of susceptibility weighted images (SWI) and high pass filtered phase images to localize and quantify brain iron. Materials and Methods Magnetic resonance (MR) images of human cadaver brain hemispheres were collected using a gradient echo based SWI sequence at 1.5T. For X-ray fluorescence (XRF) mapping, each brain was cut to obtain slices that reasonably matched the MR images and iron was mapped at the iron K-edge at 50 or 100 μm resolution. Iron was quantified using XRF calibration foils. Phase and iron XRF were averaged within anatomic regions of one slice, chosen for its range of iron concentrations and nearly perfect anatomic correspondence. X-ray absorption spectroscopy (XAS) was used to determine if the chemical form of iron was different in regions with poorer correspondence between iron and phase. Results Iron XRF maps, SWI, and high pass filtered phase data in nine brain slices from five subjects were visually very similar, particularly in high iron regions. The chemical form of iron could not explain poor matches. The correlation between the concentration of iron and phase in the cadaver brain was estimated as cFe [μg/g tissue] = 850Δφ + 110. Conclusion The phase shift Δφ was found to vary linearly with iron concentration with the best correspondence found in regions with high iron content. PMID:20512886

  15. Deformulation of a solid pharmaceutical form using computed tomography and X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Oliveira Junior, J. M.; Balcão, V. M.; Vila, M. M. D. C.; Aranha, N.; Yoshida, V. M. H.; Chaud, M. V.; Mangine Filho, S.

    2015-07-01

    Deformulation of medicines is of undeniable importance, since it can be utilized both to unravel the chemical composition of the excipients integrating a pharmaceutical formulation of a specific medicine and as an important tool to conduct morphometric studies of the formulation under study. Such strategy may be utilized in analytical studies aiming at quantifying the components of reference drugs, or in the identification of putative counterfeit pharmaceuticals. Deformulation makes use of physicochemical analysis tools to characterize, from the chemical point of view, the components integrating medicine pharmaceutical formulations and from the physical point of view, the morphological part of the pharmaceutical formulation. The techniques of computer tomography (SkyScan 1174 - Bruker microCT) and X-ray fluorescence analyses (using an X-ray source with W-anode from Hammatsu Photonics and Silicon Drift detector from Amptek) were successfully used in performing a process of deformulation of a solid pharmaceutical formulation of tablets, utilized herein as a model medicine for controlled drug release. The analytical methods used in this work, proved their effectiveness for the main goal of this study, which aimed to characterize a pharmaceutical formulation via its deconstruction.

  16. Imaging metals in proteins by combining electrophoresis with rapid x-ray fluorescence mapping.

    PubMed

    Finney, Lydia; Chishti, Yasmin; Khare, Tripti; Giometti, Carol; Levina, Aviva; Lay, Peter A; Vogt, Stefan

    2010-06-18

    Growing evidence points toward a very dynamic role for metals in biology. This suggests that physiological circumstance may mandate metal ion redistribution among ligands. This work addresses a critical need for technology that detects, identifies, and measures the metal-containing components of complex biological matrixes. We describe a direct, user-friendly approach for identifying and quantifying metal-protein adducts in complex samples using native- or SDS-PAGE, blotting, and rapid synchrotron X-ray fluorescence mapping with micro-XANES (X-ray absorption near-edge structure) of entire blots. The identification and quantification of each metal bound to a protein spot has been demonstrated, and the technique has been applied in two exemplary cases. In the first, the speciation of the in vitro binding of exogenous chromium to blood serum proteins was influenced markedly by both the oxidation state of chromium exposed to the serum proteins and the treatment conditions, which is of relevance to the biochemistry of Cr dietary supplements. In the second case, in vivo changes in endogenous metal speciation were examined to probe the influence of oxygen depletion on iron speciation in Shewanella oneidensis. PMID:20392082

  17. 3D Imaging of Transition Metals in the Zebrafish Embryo by X-ray Fluorescence Microtomography

    PubMed Central

    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

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

    SciTech Connect

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

    2013-08-15

    Purpose: To develop a proof-of-principle L-shell x-ray fluorescence (XRF) imaging system that locates and quantifies sparse concentrations of gold nanoparticles (GNPs) using a benchtop polychromatic x-ray source and a silicon (Si)-PIN diode x-ray detector system.Methods: 12-mm-diameter water-filled cylindrical tubes with GNP concentrations of 20, 10, 5, 0.5, 0.05, 0.005, and 0 mg/cm{sup 3} served as calibration phantoms. An imaging phantom was created using the same cylindrical tube but filled with tissue-equivalent gel containing structures mimicking a GNP-loaded blood vessel and approximately 1 cm{sup 3} tumor. Phantoms were irradiated by a 3-mm-diameter pencil-beam of 62 kVp x-rays filtered by 1 mm aluminum. Fluorescence/scatter photons from phantoms were detected at 90° with respect to the beam direction using a Si-PIN detector placed behind a 2.5-mm-diameter lead collimator. The imaging phantom was translated horizontally and vertically in 0.3-mm steps to image a 6 mm × 15 mm region of interest (ROI). For each phantom, the net L-shell XRF signal from GNPs was extracted from background, and then corrected for detection efficiency and in-phantom attenuation using a fluorescence-to-scatter normalization algorithm.Results: XRF measurements with calibration phantoms provided a calibration curve showing a linear relationship between corrected XRF signal and GNP mass per imaged voxel. Using the calibration curve, the detection limit (at the 95% confidence level) of the current experimental setup was estimated to be a GNP mass of 0.35 μg per imaged voxel (1.73 × 10{sup −2} cm{sup 3}). A 2D XRF map of the ROI was also successfully generated, reasonably matching the known spatial distribution as well as showing the local variation of GNP concentrations.Conclusions: L-shell XRF imaging can be a highly sensitive tool that has the capability of simultaneously imaging the spatial distribution and determining the local concentration of GNPs presented on the order of

  19. Comparison of Synchrotron X-Ray Fluorescence Mapping and Micro-XANES to Bulk X-Ray Absorption Spectra in Metal-Contaminated Sediments

    SciTech Connect

    O'Day, P; Carroll, S A; Bajt, S

    2003-01-16

    Synchrotron X-ray absorption spectroscopy (XAS) is one of the few techniques that can supply molecular-scale information for a variety of elements at concentrations relevant to natural systems in non-vacuum conditions. Bulk XAS analysis supplies the dominant chemical bonding mode(s) for a specific element. In complex materials such as natural soils and sediments, however, the dominant mode may not necessarily be the most reactive because changes in speciation at surfaces may results in changes in reactivity. Our previous work at Naval Air Station (NAS) Alameda (CA) focused on in situ metal chemistry in surface and deep sediments, and the impact of metal mobility by sediment oxidation. Estuary sediments at the Alameda Naval Station Air in California have elevated metal concentrations that increase with increasing depth. The metal concentrations in these sediments are: Cd (10-350 ppm), Cr (200-1000 ppm), Cu (100-230 ppm), Pb (200-1200 ppm) and Zn (250-600 ppm). We have extensively characterized these sediments using bulk XAS and other non-synchrotron supporting methods [ 1]. In this experiment, we collected fluorescence element maps using synchrotron X-ray microprobe of unreacted and seawater-oxidized sediment samples from Alameda NAS to determine the spatial distribution and correlation of lead, zinc, and iron. We then compared micro-XANES spectra for lead and zinc collected with the X-ray microprobe to previously collected bulk XANES spectra. The results from our bulk XAS characterization of the sediments showed both oxide and sulfide components for the trace metals. However, the bulk XAS data were not able to identify the composition of the oxide component (i.e. carbonate or hydroxide), nor could absorbed species or solid solutions be definitively identified. Our objective in using micro-XANES and fluorescence element maps was to attempt a more precise identification of metal speciation in or on individual particles.

  20. Optimizing the Operation of a Vertical Johann Spectrometer Using a High Energy Fluorescer X-ray Source

    SciTech Connect

    Haugh, Michael; Stewart, Richard

    2010-10-01

    This paper describes the operation and testing for a Vertical Johann Spectrometer (VJS) operating in the 13 keV range. The spectrometer is designed to use thin curved mica crystals or thick germanium crystals. The VJS must have a resolution E/ΔE=3000 or better to measure Doppler broadening of highly ionized krypton and operate at a small X-ray angle in order to be used as a diagnostic in a laser plasma target chamber. The VJS was aligned, tested, and optimized using a fluorescer type high energy X-ray (HEX) source located at National Security Technologies, LLC (NSTec), in Livermore, California. The HEX uses a 160 kV X-ray tube to excite fluorescence from various targets. Both rubidium and bismuth fluorescers were used for this effort. This presentation describes the NSTec HEX system and the methods used to optimize and characterize the VJS performance.

  1. Optimizing the operation of a high resolution vertical Johann spectrometer using a high energy fluorescer x-ray source

    SciTech Connect

    Haugh, Michael; Stewart, Richard

    2010-10-15

    This paper describes the operation and testing for a vertical Johann spectrometer (VJS) operating in the 13 keV range. The spectrometer is designed to use thin curved mica crystals or thick germanium crystals. The VJS must have a resolution of E/{Delta}E=3000 or better to measure the Doppler broadening of highly ionized krypton and operate at a small x-ray angle in order to be used as a diagnostic in a laser plasma target chamber. The VJS was aligned, tested, and optimized using a fluorescer type high energy x-ray (HEX) source located at National Security Technologies (NSTec), LLC, in Livermore, CA. The HEX uses a 160 kV x-ray tube to excite fluorescence from various targets. Both rubidium and bismuth fluorescers were used for this effort. This presentation describes the NSTec HEX system and the methods used to optimize and characterize the VJS performance.

  2. A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline.

    PubMed

    Fittschen, U; Guilherme, A; Böttger, S; Rosenberg, D; Menzel, M; Jansen, W; Busker, M; Gotlib, Z P; Radtke, M; Riesemeier, H; Wobrauschek, P; Streli, C

    2016-05-01

    An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml(-1) to µg ml(-1)). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NIST water 1640. Low limits of detection of less than 100 fg absolute (10 pg ml(-1)) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. PMID:27140163

  3. Remote analyses of highly radioactive samples by x-ray fluorescence

    SciTech Connect

    Warrant, R.W.; Shurtliff, R.M.; Haskell, K.J.; Ryder, W.A.

    1991-09-11

    The Idaho Chemical Processing Plant (ICPP) is a multipurpose nuclear fuel and waste processing facility located at the Idaho National Engineering Laboratory (INEL) near Idaho Falls, Idaho. The plant is presently operated for the Department of Energy (DOE) by a subsidiary of Westinghouse Electric Company, Westinghouse Idaho Nuclear Company (WINCO). The facility receives and processes a large variety of reactor fuel types. The analysis of spent nuclear fuel reprocessing streams causes some unique problems for the analytical chemist. The major problems are the high levels of radioactivity, the complex solution of fuel components, fission products, dissolved cladding, and dissolver solutions as well as the need for rapid results. For the analysis of the heavy metals in these complex radioactive samples, the technique of wavelength dispersive X-ray fluorescence offers some distinct advantages. The method is specific, highly automated, and the sample requires minimum preparation.

  4. In vivo X-ray fluorescence estimation of bone lead concentrations in Queensland adults.

    PubMed

    Price, J; Baddeley, H; Kenardy, J A; Thomas, B J; Thomas, B W

    1984-01-01

    A group of 200 Queensland adults without known health problems had in-vivo estimation of finger bone lead concentrations using X-ray fluorescence analysis (XRF). Forty of these subjects had elevated levels of bone lead of 25 ppm or more, consistent with exposure to the metal. Although the correlation between Queensland residence during childhood and raised bone lead levels was not significant, there were significant correlations between childhood residence in a painted wooden house and raised levels, and between occupational exposure and raised levels. Of the 40 subjects with elevated lead levels only two had neither a history of occupational exposure or childhood residence in a wooden house, whereas 11 of the 25 who had a history of both occupational and residential exposure were positive. The data are consistent with lead in housepaint, or absorbed during occupational exposure, being the two major sources of raised bone lead concentrations. PMID:6704645

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

    PubMed

    Wang, Zhi-gang; Yu, Hong-mei

    2012-01-01

    The content of the elements C, H, O and N in Jinhua bergamot was analysed by using Vario III elemental analyser, the bergamot sample was scanned by using X-ray fluorescence spectrometer with PW2400 wavelength dispersion, and the content of the elements Mg, Al, P, S, Cl, K, Ca, Mn, Fe and Sr was analysed by using IQ+ analytical method. It turned out that the result is more ideal if the content of the elements C, H, O and N is processed as fix phase, and the analytical result is more ideal if, to prevent the sample skin from coming off, the sample is wrapped with mylar film with the film coefficient adjusted. PMID:22497170

  6. Determination of silicon in organic matrices with grazing-emission X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Claes, M.; Van Dyck, K.; Deelstra, H.; Van Grieken, R.

    1999-10-01

    The potential of a prototype grazing-emission X-ray fluorescence spectrometer for reliable analysis of sample solutions, obtained by pressurized microwave oven digestion of Si-spiked organic and biological materials, was investigated as part of an inter-laboratory study. The fact that this grazing-emission technique is based on the total reflection phenomenon and wavelength-dispersive detection, gives it the benefit to determine light elements in a sensitive way. Results of the determination of silicon in pork liver, cellulose, urine, serum, spinach, beer, mineral water and horsetail (dry plant extract) samples are presented. Some of the results are compared with those obtained with other analytical techniques. The study proved that determination of silicon traces in biological matrices represents an extremely difficult task, however, measurements of silicon are achieved with acceptable precision. The most important problems still arise when sample pre-treatment is needed prior to analysis.

  7. Possible use of pattern recognition for the analysis of Mars rover X-ray fluorescence spectra

    NASA Technical Reports Server (NTRS)

    Yin, Lo I; Trombka, Jacob I.; Seltzer, Stephen M.; Johnson, Robert G.; Philpotts, John A.

    1989-01-01

    On the Mars rover sample-return mission, the rover vehicle will collect and select samples from different locations on the Martian surface to be brought back to earth for laboratory studies. It is anticipated that an in situ energy-dispersive X-ray fluorescence (XRF) spectrometer will be on board the rover. On such a mission, sample selection is of higher priority than in situ quantitative chemical anlaysis. With this in mind, a pattern recognition technique is proposed as a simple, direct, and speedy alternative to detailed chemical analysis of the XRF spectra. The validity and efficacy of the pattern recognition technique are demonstrated by the analyses of laboratory XRF spectra obtained from a series of geological samples, in the form both of standardized pressed pellets and as unprepared rocks. It is found that pattern recognition techniques applied to the raw XRF spectra can provide for the same discrimination among samples as a knowledge of their actual chemical composition.

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  9. Determination of thorium in geological materials by x-ray fluorescence spectrometry after anion exchange extraction

    SciTech Connect

    Roelandts, I.

    1983-08-01

    The exchange capacity of the resin was determined to be 1 m equiv of Th/g dry resin. Synthetic calibration standards of thorium were prepared over a large concentration range, for use as an independent method of calibration. The advantages and disadvantages of direct x-ray fluorescence analysis are discussed. The lower limit of detection has been calculated according to Currie's convention and was found to be equal to 13 ..mu..g of Th/250 mg of resin, sufficient for the range of concentrations found in Th bearing minerals and ores. Results using Canadian syenite rocks and a suite of South African reference minerals show that the proposed method appears to be relatively precise and accurate for exploration geochemistry. 1 figure, 2 tables.

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

    NASA Technical Reports Server (NTRS)

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

    2008-01-01

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

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

    SciTech Connect

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

    1990-08-01

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

  12. Validation of X-ray fluorescence spectrometry for determining osseous or dental origin of unknown material.

    PubMed

    Christensen, Angi M; Smith, Michael A; Thomas, Richard M

    2012-01-01

    Forensic anthropological examinations typically involve the analysis of human skeletal remains, but in cases where samples are very small and/or physically compromised, it may first be necessary to determine whether the material is even osseous or dental in origin. X-ray fluorescence spectrometry (XRF) is a technique that reveals the elemental composition of materials and is hypothesized to have utility in such cases. XRF analysis was conducted on a variety of tissues and materials in unaltered and altered (damaged) states. With few exceptions, osseous and dental tissues in unaltered and altered conditions contained characteristic levels of calcium and phosphorus, while other materials did not. Materials could be accurately identified as osseous or dental in origin based on the calcium and phosphorus levels identified by XRF, and we therefore conclude that XRF analysis is a valid and effective means of determining osseous or dental origin of unknown material. PMID:22040159

  13. Dependence of X-Ray fluorescence intensity on sample specific gravity

    SciTech Connect

    Az'muko, A.A.; Butuina, L.F.; Smagunova, A.N.; Tarasenko, S.V.

    1986-06-01

    In order to understand the physical nature of the experimental relation I=f(n), the authors set up tests that study the dependence of intensity on packing density. Tests were carried out on samples of the minerals galena cassiterite, and zircon, and cassiterite-calcite and zircon-quartz mixtures. The intensities of the Pb L Sn K /SUB alpha/ , and Zr K /SUB alpha/ lines were measured in a KRFS-5 spectrometer with BKhV-6 x-ray tube with tungsten anode. The experimental and theoretical functions I /SUB rel/ =fIn) for galena are shown and the values of the effect understudy are given. It is shown that the observed dependence of fluorescence intensity on sample density is due to the effect of sample surface quality on the value of I /SUB A/ .

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

    NASA Technical Reports Server (NTRS)

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

    1977-01-01

    The X-ray spectrum of Hercules X-1 was observed in the energy range 2-24 keV from August 29 to September 3, 1975. A broad iron line feature is observed in the normal high state spectrum. The line equivalent width is given along with its full-width-half-maximum energy. Iron line fluorescence from an opaque, cool shell of material at the Alfven surface provides the necessary luminosity in this feature. The line energy width can be due to Doppler broadening if the shell is forced to corotate with the pulsar at a radius 800 million cm. Implications of this model regarding physical conditions near Her X-1 are discussed.

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

    NASA Technical Reports Server (NTRS)

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

    1986-01-01

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

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

    NASA Astrophysics Data System (ADS)

    Popescu, Bogdan F. Gh; George, Martin J.; Bergmann, Uwe; Garachtchenko, Alex V.; Kelly, Michael E.; McCrea, Richard P. E.; Lüning, Katharina; Devon, Richard M.; George, Graham N.; Hanson, Akela D.; Harder, Sheri M.; Chapman, L. Dean; Pickering, Ingrid J.; Nichol, Helen

    2009-02-01

    Rapid-scanning x-ray fluorescence (RS-XRF) is a synchrotron technology that maps multiple metals in tissues by employing unique hardware and software to increase scanning speed. RS-XRF was validated by mapping and quantifying iron, zinc and copper in brain slices from Parkinson's disease (PD) and unaffected subjects. Regions and structures in the brain were readily identified by their metal complement and each metal had a unique distribution. Many zinc-rich brain regions were low in iron and vice versa. The location and amount of iron in brain regions known to be affected in PD agreed with analyses using other methods. Sample preparation is simple and standard formalin-fixed autopsy slices are suitable. RS-XRF can simultaneously and non-destructively map and quantify multiple metals and holds great promise to reveal metal pathologies associated with PD and other neurodegenerative diseases as well as diseases of metal metabolism.

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

    SciTech Connect

    Tellería Narvaez, C.A.; Fernández Alcázar, S.; Barrientos Zamora, F.G.; Chungara Castro, J.; Luna Lauracia, I.; Mamani Tola, H.; Mita Peralta, E.; Muñoz Gosálvez, A.O.; Romero Bolaños, L.E.; Ramírez Ávila, G.M.

    2014-06-15

    As a first step in the evaluation of nutritional levels in Bolivian children (8–13 years-old), we carried out X-Ray Fluorescence measurements in hair samples of children belonging to different social classes and living either in rural areas or in cities. The aim of this study is to contribute to health policies tending to improve the global health of children and consequently avoid malnutrition. Our method intends to have maximum reliability and at the same time be as simple as possible from an experimental point of view. Additionally, we use this method to determine some other elements such as Fe, Cu, Pb, As and Hg, the latter three considered as contaminants that could be present in children living in areas which neighbor mines and industries. This work will be complemented by some biological and medical tests.

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

    NASA Astrophysics Data System (ADS)

    Tellería Narvaez, C. A.; Fernández Alcázar, S.; Barrientos Zamora, F. G.; Chungara Castro, J.; Luna Lauracia, I.; Mamani Tola, H.; Mita Peralta, E.; Muñoz Gosálvez, A. O.; Romero Bolaños, L. E.; Ramírez Ávila, G. M.

    2014-06-01

    As a first step in the evaluation of nutritional levels in Bolivian children (8-13 years-old), we carried out X-Ray Fluorescence measurements in hair samples of children belonging to different social classes and living either in rural areas or in cities. The aim of this study is to contribute to health policies tending to improve the global health of children and consequently avoid malnutrition. Our method intends to have maximum reliability and at the same time be as simple as possible from an experimental point of view. Additionally, we use this method to determine some other elements such as Fe, Cu, Pb, As and Hg, the latter three considered as contaminants that could be present in children living in areas which neighbor mines and industries. This work will be complemented by some biological and medical tests.

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

    PubMed

    Gilpin, Megan; Christensen, Angi M

    2015-07-01

    Analyzing and identifying skeletal remains becomes increasingly difficult when remains have been cremated, especially in cases where the cremated material may have been intentionally contaminated with nonskeletal material. This study examined the potential of X-ray fluorescence spectrometry (XRF) to detect the presence of nonskeletal contaminants in samples of cremains. Eleven samples of cremains were variably combined with concrete mix and analyzed using XRF. Photon counts of elements in each sample were analyzed, and the coefficient of determination (R(2)) using unweighted linear regression as a function of percent cremains was calculated. Results showed that with changes in the proportion of skeletal material and contaminant, there were significant (R(2) > 0.90) changes in detected levels of phosphorus, potassium, zinc, aluminum, and sulfur. The use of XRF is concluded to be a valid approach in the identification of the presence of nonskeletal material in potentially contaminated cremains. PMID:25762496

  20. Unique Properties of Thermally Tailored Copper: Magnetically Active Regions and Anomalous X-ray Fluorescence Emissions

    PubMed Central

    2009-01-01

    When high-purity copper (≥99.98%wt) is melted, held in its liquid state for a few hours with iterative thermal cycling, then allowed to resolidify, the ingot surface is found to have many small regions that are magnetically active. X-ray fluorescence analysis of these regions exhibit remarkably intense lines from “sensitized elements” (SE), including in part or fully the contiguous series V, Cr, Mn, Fe, and Co. The XRF emissions from SE are far more intense than expected from known impurity levels. Comparison with blanks and standards show that the thermal “tailoring” also introduces strongly enhanced SE emissions in samples taken from the interior of the copper ingots. For some magnetic regions, the location as well as the SE emissions, although persistent, vary irregularly with time. Also, for some regions extraordinarily intense “sensitized iron” (SFe) emissions occur, accompanied by drastic attenuation of Cu emissions. PMID:20037657

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

    SciTech Connect

    Bunn, Amoret L.; Fritz, Brad G.; Wellman, Dawn M.

    2014-07-15

    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.

  2. Evaluation on determination of iodine in coal by energy dispersive X-ray fluorescence

    USGS Publications Warehouse

    Wang, B.; Jackson, J.C.; Palmer, C.; Zheng, B.; Finkelman, R.B.

    2005-01-01

    A quick and inexpensive method of relative high iodine determination from coal samples was evaluated. Energy dispersive X-ray fluorescence (EDXRF) provided a detection limit of about 14 ppm (3 times of standard deviations of the blank sample), without any complex sample preparation. An analytical relative standard deviation of 16% was readily attainable for coal samples. Under optimum conditions, coal samples with iodine concentrations higher than 5 ppm can be determined using this EDXRF method. For the time being, due to the general iodine concentrations of coal samples lower than 5 ppm, except for some high iodine content coal, this method can not effectively been used for iodine determination. More work needed to meet the requirement of determination of iodine from coal samples for this method. Copyright ?? 2005 by The Geochemical Society of Japan.

  3. Application of x-ray fluorescence analysis to investigation of the composition of gunshot residues

    NASA Astrophysics Data System (ADS)

    Kazimirov, V. I.; Zorin, A. D.; Zanozina, V. F.

    2006-05-01

    We have used x-ray fluorescence analysis to study the elemental composition of gunshot residues from smooth-bore and rifled-bore guns. We have established that it is possible to differentiate between types of projectiles (jacketed/lead), types of primers (corrosive/noncorrosive), and types of propellant powders (black/smokeless) by analysis of the elemental composition of the gunshot residues. We have shown that the mercury content in gunshot residues on the surface of the object carrying the residues steadily decreases as storage time increases. Despite this fact, mercury can be preserved as a component of gunshot residues on the object (cotton cloth) under room conditions for more than 45 days.

  4. Micro-x-ray fluorescence, micro-x-ray absorption spectroscopy, and micro-x-ray diffraction investigation of lead speciation after the addition of different phosphorus amendments to a smelter-contaminated soil.

    PubMed

    Baker, Lucas R; Pierzynski, Gary M; Hettiarachchi, Ganga M; Scheckel, Kirk G; Newville, Matthew

    2014-03-01

    The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that the differences in the efficacy of Pb stabilization in contaminated soils on fluid or granular P amendment addition is due to different P reaction processes in and around fertilizer granules and fluid droplets. We used a combination of several synchrotron-based techniques (i.e., spatially resolved micro-X-ray fluorescence, micro-X-ray absorption near-edge structure spectroscopy, and micro-X-ray diffraction) to speciate Pb at two incubation times in a smelter-contaminated soil on addition of several fluid and granular P amendments. The results indicated that the Pb phosphate mineral plumbogummite was an intermediate phase of pyromorphite formation. Additionally, all fluid and granular P sources were able to induce Pb phosphate formation, but fluid phosphoric acid (PA) was the most effective with time and distance from the treatment. Granular phosphate rock and triple super phosphate (TSP) amendments reacted to generate Pb phosphate minerals, with TSP being more effective at greater distances from the point of application. As a result, PA and TSP were the most effective P amendments at inducing Pb phosphate formation, but caution needs to be exercised when adding large amounts of soluble P to the environment. PMID:25602650

  5. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    NASA Astrophysics Data System (ADS)

    Fernández-Ruiz, R.; García-Heras, M.

    2007-10-01

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications.

  6. The reproducibility of [sup 109]Cd-based X-ray fluorescence measurements of bone lead

    SciTech Connect

    Gordon, C.L. ); Webber, C.E.; Chettle, D.R. )

    1994-08-01

    We assessed the reproducibility of X-ray fluorescence-based lead measurements from multiple measurements made on a low-concentration plaster of paris phantom and in five subjects measured five times on two occasions. Over a 6-month period, 220 measurements of the same phantom were obtained and showed a standard deviation of 1.29 [mu]g Pb (g plaster of paris)[sup [minus]1]. The two sets of in vivo measurements were made 10 months apart and revealed a mean standard deviation of 3.4 [mu]Pb (g bone mineral)[sup [minus]1] and 5.1 [mu]g Pb (g bone mineral)[sup [minus]1] for males and females, respectively. Our measured standard deviation exceeded by 20-30% the calculated standard deviation associated with a single measurement both in the phantom and in subjects. This indicates that some variance is introduced during the measurement process. Operator learning and consistency significantly minimized this increased variability. Measured lead concentrations of the left and right tibia in 14 subjects showed no significant differences between legs. As a result, either tibia can be sampled and compared over time. The levels of reproducibility we report here mean that X-ray fluorescence-based determinations of bone lead concentrations are reliable both over the short and long term. Thus, reasonably sized confidence intervals can be placed on detected changes in concentration and should permit acquisition of longitudinal data within a reasonable length of time. 19 refs., 1 fig., 6 tabs.

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

    NASA Astrophysics Data System (ADS)

    Chtcheprov, Pavel; Inscoe, Christina; Burk, Laurel; Ger, Rachel; Yuan, Hong; Lu, Jianping; Chang, Sha; Zhou, Otto

    2014-03-01

    Microbeam radiation therapy (MRT) uses an array of high-dose, narrow (~100 μm) beams separated by a fraction of a millimeter to treat various radio-resistant, deep-seated tumors. MRT has been shown to spare normal tissue up to 1000 Gy of entrance dose while still being highly tumoricidal. Current methods of tumor localization for our MRT treatments require MRI and X-ray imaging with subject motion and image registration that contribute to the measurement error. The purpose of this study is to develop a novel form of imaging to quickly and accurately assist in high resolution target positioning for MRT treatments using X-ray fluorescence (XRF). The key to this method is using the microbeam to both treat and image. High Z contrast media is injected into the phantom or blood pool of the subject prior to imaging. Using a collimated spectrum analyzer, the region of interest is scanned through the MRT beam and the fluorescence signal is recorded for each slice. The signal can be processed to show vascular differences in the tissue and isolate tumor regions. Using the radiation therapy source as the imaging source, repositioning and registration errors are eliminated. A phantom study showed that a spatial resolution of a fraction of microbeam width can be achieved by precision translation of the mouse stage. Preliminary results from an animal study showed accurate iodine profusion, confirmed by CT. The proposed image guidance method, using XRF to locate and ablate tumors, can be used as a fast and accurate MRT treatment planning system.

  8. [Determination of major elements in superphosphate by X-ray fluorescence spectrometry].

    PubMed

    Rui, Yu-Kui; Li, He; Shen, Jian-Bo; Zhang, Fu-Suo

    2008-11-01

    Phosphate fertilizer is one of the most important fertilizers. The authors determined nine kinds of major elements in superphosphate, the most important phosphate fertilizer, by X-ray fluorescence spectrometry. The detection range of SiO2, Al2O3, TFe2O3, MnO, MgO, CaO, Na2O, K2O and P2O5 is 15.0%-90.0%, 0.20%-25.0%, 0.20%-25.0%, 0.01%-0.35%, 0.20%-40.0%, 0.10%-35.0%, 0.10%-7.50%, 0.05%-7.50% and 1.00%-100.00% respectively, and the precision of the method for SiO2, Al2O3, TFe2O3, MnO, MgO, CaO, Na2O, K2O and P2O5 range from 0.20% to 0.005%, so the method of X-ray fluorescence spectrometry is a fast and effectual method for detecting the composition of phosphate fertilizer. The contents of the above elements showed (1) the detected superphosphate content is 18.101% of P2O5, which is accordant to the labeled level (> or = 16%); (2) the detected superphosphate contains much SiO2, TFe2O3, MgO, CaO and K2O, which are necessary for plant growth and the content of which is 16.954%, 1.495%, 1.580%, 21.428% and 1.585% respectively. These data showed that phosphate fertilizer sometimes can supply some trace elements for plants, but we should eliminate the interference effect of these elements when we research the role of phosphorus; (3) superphosphate contains 3.225% of Al2O3, so the authors should attention to the aluminium poison when superphosphate is used chronically. PMID:19271522

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

    NASA Astrophysics Data System (ADS)

    O'Brien, S. L.; Whiteside, M. D.; Sholto-Douglas, D.; Dohnalkova, A.; Durall, D. M.; Gursoy, D.; Jones, M. D.; Kovarik, L.; Lai, B.; Roehrig, C.; Sullivan, S.; Vogt, S.; Kemner, K. M.

    2015-12-01

    The metabolic activities of soil microbes are the primary drivers of biogeochemical processes controlling the terrestrial carbon cycle, nutrient availability to plants, contaminant remediation, water quality, and other ecosystem services. However, we have a limited understanding of microbial metabolic processes such as nutrient uptake rates, substrate preferences, or how microbes and microbial metabolism are distributed throughout the three-dimensional pore network of the soil. Here we use a novel combination of imaging techniques with quantum dots (QDs, engineered semiconductor nanoparticles that produce size or composition-dependent fluorescence) to locate bacteria in the three-dimensional pore network of a soil aggregate. First, we show using confocal and aberration-corrected transmission electron microscopies that bacteria (Bacillus subtilis, Pseudomonas fluorescens, and Pseudomonas protogens) actively take up and internalize CdSe/ZnS core/shell QDs conjugated to biologically relevant substrates. Next, we show that cells bearing QDs can be identified using fluorescence imaging with hard x-rays at 2ID-D at the Advanced Photon Source (APS). Finally, we demonstrate that the Se constituent to the QDs can be used to label bacteria in three-dimensional tomographic reconstructions of natural soil at 0.5 nm spatial resolution using hard x-rays at 2ID-E at the APS. This is the first time soil bacteria have been imaged in the intact soil matrix at such high resolution. These results offer a new way to experimentally investigate basic bacterial ecology in situ, revealing constraints on microbial function in soil that will help improve connections between pore-scale and ecosystem-scale processes in models.

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

    PubMed

    Gallardo, Helena; Queralt, Ignasi; Tapias, Josefina; Candela, Lucila; Margui, Eva

    2016-08-01

    Monitoring total bromine and bromide concentrations in soils is significant in many environmental studies. Thus fast analytical methodologies that entail simple sample preparation and low-cost analyses are desired. In the present work, the possibilities and drawbacks of low-power total reflection X-ray fluorescence spectrometry (TXRF) for the determination of total bromine and bromide contents in soils were evaluated. The direct analysis of a solid suspension using 20 mg of fine ground soil (<63 μm) gave a 3.7 mg kg(-1) limit of detection for bromine which, in most cases, was suitable for monitoring total bromine content in soils (Br content range in soils = 5-40 mg kg(-1)). Information about bromide determination in soils is also possible by analyzing the Br content in water soil extracts. In this case, the TXRF analysis can be directly performed by depositing 10 μL of the internal standardized soil extract sample on a quartz glass reflector in a measuring time of 1500 s. The bromide limit of detection by this approach was 10 μg L(-1). Good agreement was obtained between the TXRF results for the total bromine and bromide determinations in soils and those obtained by other popular analytical techniques, e.g. energy dispersive X-ray fluorescence spectrometry (total bromine) and ionic chromatography (bromide). As a study case, the TXRF method was applied to study bromine accumulation in two agricultural soils fumigated with a methyl bromide pesticide and irrigated with regenerated waste water. PMID:27179429

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

    PubMed Central

    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.

    2014-01-01

    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 Cln6nclf (CbCln6nclf) 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 CbCln6nclf cells. Subtle differences in the zinc K-edge X-ray Absorption Near Edge Structure (XANES) spectra of control and CbCln6nclf cells suggested that impaired zinc homeostasis may be associated with an altered ligand set in CbCln6nclf cells. Importantly, a zinc-complex, ZnII(atsm), restored the nuclear-to-cytoplasmic zinc ratios in CbCln6nclf cells via nuclear zinc delivery, and restored the relationship between subcellular zinc and calcium levels to that observed in healthy control cells. ZnII(atsm) treatment also resulted in a reduction in the

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

    PubMed

    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

  13. 2D/3D cryo x-ray fluorescence imaging at the bionanoprobe at the advanced photon source

    NASA Astrophysics Data System (ADS)

    Chen, S.; Paunesku, T.; Yuan, Y.; Deng, J.; Jin, Q.; Hong, Y. P.; Vine, D. J.; Lai, B.; Flachenecker, C.; Hornberger, B.; Brister, K.; Jacobsen, C.; Woloschak, G. E.; Vogt, S.

    2016-01-01

    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.

  14. Multi-element analysis of pyrite ores using polarized energy-dispersive X-ray fluorescence spectrometry.

    PubMed

    Ustündağ, Zafer; Ustündağ, Ilknur; Kağan Kadioğlu, Yusuf

    2007-07-01

    X-ray fluorescence (XRF) spectrometry is used worldwide in geological material analysis. This study, applies polarized energy-dispersive X-ray fluorescence (PEDXRF) Spectrometer and compares in the samples of Rize-Cayeli and Mardin pyrite ores. The samples of pyrite ore were collected from the Rize and Mardin in Turkey. The prepared samples were analyzed using a PEDXRF spectrometer. The result of the analysis shows the presence of many elements including rare-earth elements (from Na to Th). The accuracy and precision of the technique for chemical analysis is demonstrated by analyzing USGS standards, GEOL, GBW 7109 and GBW-7309 sediment. PMID:17459714

  15. [Energy-dispersive x-ray fluorescence spectrometry--a forensic chemistry method for determination of shooting distance].

    PubMed

    Havel, J

    2003-10-01

    The article follows up the experiences Energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic necrochemical method as the tool for detection of metals (gunshot residues--GSR) in connection with gunshot-wounds of persons--authors: dipl. Ing. J. Havel and dipl. Ing. K. Zelenka and Energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic method as the tool for identification of inlets (gunshot--entries) and outlets (gunshot--exits)--author: dipl. Ing. J. Havel. PMID:14661530

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  17. Reconstruction of Elemental Distribution Images from Synchrotron Radiation X-Ray Fluorescence Spectra

    NASA Astrophysics Data System (ADS)

    Toque, Jay Arre; Ide-Ektessabi, Ari

    Synchrotron radiation X-ray fluorescence spectroscopy (SRXRF) is a powerful technique for studying trace elements in biological samples and other materials in general. Its features including capability to perform measurements in air and water, noncontact and nondestructive assay are superior to other elemental analysis techniques. In this study, a technique for reconstructing elemental distribution mapping of trace elements from spectral data was developed. The reconstruction was made possible by using the measured fluorescent signals to obtain local differences in elemental concentrations. The proposed technique features interpolation and background subtraction using matrix transformations of the spectral data to produce an enhanced distribution images. It is achieved by employing polychromatic or monochromatic color assignments proportional to the fluorescence intensities for displaying single-element or multiple-element distributions respectively. Some typical applications (i.e., macrophage and tissue surrounding an implant) were presented and the samples were imaged using the proposed method. The distribution images of the trace elements of the selected samples were used in conjunction with other analytical techniques to draw relevant observations, which cannot be achieved using conventional techniques such as metallic uptake and corresponding cellular response. The elemental distribution images produced from this study were found to have better quality compared to images produced using other analytical techniques (e.g., SIMS, PIXE, XPS, etc).

  18. Trace Element Mapping of a Biological Specimen by a Full-Field X-ray Fluorescence Imaging Microscope with a Wolter Mirror

    SciTech Connect

    Hoshino, Masato; Yamada, Norimitsu; Ishino, Toyoaki; Namiki, Takashi; Watanabe, Norio; Aoki, Sadao

    2007-01-19

    A full-field X-ray fluorescence imaging microscope with a Wolter mirror was applied to the element mapping of alfalfa seeds. The X-ray fluorescence microscope was built at the Photon Factory BL3C2 (KEK). X-ray fluorescence images of several growing stages of the alfalfa seeds were obtained. X-ray fluorescence energy spectra were measured with either a solid state detector or a CCD photon counting method. The element distributions of iron and zinc which were included in the seeds were obtained using a photon counting method.

  19. Determination of heavy metals in suspended waste water collected from Oued El Harrach Algiers River by Energy Dispersive X-Ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Ouziane, S.; Amokrane, A.; Toumert, I.

    2013-12-01

    A preliminary study of the atmospheric pollution in the centre of Algiers is one of the important fields of applications in the environmental science. Nowadays, we need to evaluate the level of the contamination which has an unfavourable effect on physicochemical properties of soils and plants and namely also on human health. In the present work, water samples collected from Oued El-Harrach Algiers River, have been filtered in 0.45 μm Millipore filters to be analysed by Energy Dispersive X-Ray Fluorescence technique using 109Cd radioisotope source. Concentrations of the toxic elements like heavy metals are determined and compared with the published ones values by Yoshida [1] and those obtained using PIXE and NAA techniques [6].

  20. Distribution and speciation of bromine in mammalian tissue and fluids by X-ray fluorescence imaging and X-ray absorption spectroscopy.

    PubMed

    Ceko, Melanie J; Hummitzsch, Katja; Hatzirodos, Nicholas; Bonner, Wendy; James, Simon A; Kirby, Jason K; Rodgers, Raymond J; Harris, Hugh H

    2015-05-01

    Bromine is one of the most abundant and ubiquitous trace elements in the biosphere and until recently had not been shown to perform any essential biological function in animals. A recent study demonstrated that bromine is required as a cofactor for peroxidasin-catalysed formation of sulfilimine crosslinks in Drosophila. In addition, bromine dietary deficiency is lethal in Drosophila, whereas bromine replenishment restores viability. The aim of this study was to examine the distribution and speciation of bromine in mammalian tissues and fluids to provide further insights into the role and function of this element in biological systems. In this study we used X-ray fluorescence (XRF) imaging and inductively coupled plasma-mass spectrometry (ICP-MS) to examine the distribution of bromine in bovine ovarian tissue samples, follicular fluid and aortic serum, as well as human whole blood and serum and X-ray absorption spectroscopy (XAS) to identify the chemical species of bromine in a range of mammalian tissue (bovine, ovine, porcine and murine), whole blood and serum samples (bovine, ovine, porcine, murine and human), and marine samples (salmon (Salmo salar), kingfish (Seriola lalandi) and Scleractinian coral). Bromine was found to be widely distributed across all tissues and fluids examined. In the bovine ovary in particular it was more concentrated in the sub-endothelial regions of arterioles. Statistical comparison of the near-edge region of the X-ray absorption spectra with a library of bromine standards led to the conclusion that the major form of bromine in all samples analysed was bromide. PMID:25675086

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

    PubMed Central

    de Jonge, Martin D.; Ryan, Christopher G.; Jacobsen, Chris J.

    2014-01-01

    X-ray nanoprobes require coherent illumination to achieve optic-limited resolution, and so will benefit directly from diffraction-limited storage rings. Here, the example of high-resolution X-ray fluorescence tomography is focused on as one of the most voracious demanders of coherent photons, since the detected signal is only a small fraction of the incident flux. Alternative schemes are considered for beam delivery, sample scanning and detectors. One must consider as well the steps before and after the X-ray experiment: sample preparation and examination conditions, and analysis complexity due to minimum dose requirements and self-absorption. By understanding the requirements and opportunities for nanoscale fluorescence tomography, one gains insight into the R&D challenges in optics and instrumentation needed to fully exploit the source advances that diffraction-limited storage rings offer. PMID:25177992

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

    NASA Astrophysics Data System (ADS)

    Polgári, Zs.; Meirer, F.; Sasamori, S.; Ingerle, D.; Pepponi, G.; Streli, C.; Rickers, K.; Réti, A.; Budai, B.; Szoboszlai, N.; Záray, G.

    2011-03-01

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

  3. Silver speciation in liver of marine mammals by synchrotron X-ray absorption fine structure and X-ray fluorescence spectroscopies.

    PubMed

    Nakazawa, Emiko; Ikemoto, Tokutaka; Hokura, Akiko; Terada, Yasuko; Kunito, Takashi; Yamamoto, Takahito; Yamada, Tadasu K; Rosas, Fernando C W; Fillmann, Gilberto; Tanabe, Shinsuke; Nakai, Izumi

    2011-06-01

    The chemical form of Ag in the livers of five species of marine mammals was examined using X-ray absorption fine structure (XAFS) and X-ray fluorescence (XRF) spectroscopies. The XAFS analysis suggested that Ag(2)Se was present in the livers of the Franciscana dolphin (Pontoporia blainvillei), Dall's porpoise (Phocoenoides dalli), and Baird's beaked whale (Berardius bairdii), whereas Ag(2)S was present in the livers of the striped dolphin (Stenella coeruleoalba) and pygmy killer whale (Feresa attenuata). XRF spectroscopy results revealed that the distribution patterns of Ag and Se in a thin section of the liver of the Franciscana dolphin were the same; this also implied that Ag was associated with Se in the liver. Thus, the interaction of Ag with Se or S may offer significant protection against the toxicity of Ag in marine mammals. The formation of either Ag(2)Se or Ag(2)S might depend on the Hg levels in the liver. Ag(2)Se was observed in liver samples with relatively high Ag/Hg ratio, whereas liver samples with low Ag/Hg ratio contained Ag(2)S. PMID:21491037

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

    NASA Astrophysics Data System (ADS)

    Prandel, L. V.; Saab, S. C.; Brinatti, A. M.; Giarola, N. F. B.; Leite, W. C.; Cassaro, F. A. M.

    2014-02-01

    Diffraction and spectroscopic techniques have been shown to be suitable for obtaining physical and mineralogical properties in polycrystalline soil samples, and also in their precursor compounds. For instance, the X-ray fluorescence (XRF) spectroscopy allows obtaining the elemental composition of an investigated sample, while the X-ray diffraction (XRD) technique permits obtaining qualitative and quantitative composition of the soil minerals through the Rietveld method (RM). In this study Yellow Latosol (Oxisol), Yellow Argisol (Ultisol) and Gray Argisol (Ultisol) soil samples, classified as "hardsetting soils", extracted from areas located at Northeast and Southeast of Brazilian coast were investigated. The soils and their fractions were analyzed in an EDX-700 and an XRD-6000 (Cu Kα radiation). XRF results indicate high percentages of Si and Al, and small percentage of Fe and Ti in the investigated samples. The DRX data and RM indicate that there was a predominance of kaolinite and halloysite minerals (kaolin group minerals) in the clay fractions, which are presumably responsible for the formation of kaolinitic plasma in these soils. Also, the obtained results showed that the XRF, XRD techniques and RM were very helpful for investigating the mineralogical composition of a hardsetting soil.

  5. Sulfur abundance of asteroid 25143 Itokawa observed by X-ray fluorescence spectrometer onboard Hayabusa

    NASA Astrophysics Data System (ADS)

    Arai, Takehiko; Okada, Tatsuaki; Yamamoto, Yukio; Ogawa, Kazunori; Shirai, Kei; Kato, Manabu

    2008-01-01

    The Japanese Hayabusa spacecraft successfully carried out in situ observations of S-class asteroid 25143 Itokawa, including the surface major elemental analysis with the X-ray fluorescence spectrometer (XRSHayabusa). Our previous results for the X-ray experiments (Okada et al., 2006a) indicated that major elemental ratios of Mg/Si and Al/Si on the surface of Itokawa resemble ordinary LL- or L-chondrites more than any other meteorite analogues. In the NEAR Shoemaker observations of S-class asteroid 433 Eros, the results of X-ray fluorescence observations indicated the depletion of sulfur, probably reflecting impact-induced volatilization, photoor ion-induced sputtering at the surface, or the loss of FeS-rich materials due to partial melting. Here, we determined the elemental abundance of sulfur (S) on the surface of Itokawa, in addition to that of Mg, Al, and Si, and its regional variation using XRS-Hayabusa observations. In particular, we carefully corrected the fluctuation of solar X-rays, variation of surface geometry, and sensor response function in this analysis, and thus we believe that the results are more accurate than those of our previous report. In this study, the upper and lower limits for Mg/Si, Al/Si, and S/Si overlap those of meteorite analogues for ordinary chondrites or primitive achondrites. In terms of the major elemental composition, Itokawa is best classified as a ordinary chondrite or a primitive achondrite. Our models do not include the mineral mixing effects. With the effects, the abundance of sulfur is expected to be 30% lower than our results. Hence, we conclude that the abundance of sulfur on the surface of Itokawa is almost equal to or even lower than the average abundance in ordinary chondrites. Although the abundances for Mg and Si are globally homogeneous, best-fit or upper limits of mass fraction for Al and S vary in local areas. There is a negative correlation (-0.92) for Al/Si vs. S/Si in ten facets. In particular, the area with the

  6. X-Ray Fluorescence Solvent Detection at the Substrate-Adhesive Interface

    NASA Technical Reports Server (NTRS)

    Wurth, Laura; Evans, Kurt; Weber, Bart; Headrick, Sarah

    2005-01-01

    tag element can then be mapped by its characteristic x-ray emission using either x-ray fluorescence, or electron-beam energy-and wavelength-dispersive x-ray spectrometry. The direct mapping techniques avoid issues of different diffusion or migration rates of solvents and elemental tags, while the indirect techniques avoid spectral resolution issues in cases where solvents and substrates have adjacent or overlapping peaks. In this study, cross-section component indirect mapping is being evaluated as a method for measuring migration of d-limonene based solvents in glass-cloth phenolic composite (GCP) prior to and during subsequent bonding and epoxy adhesive cure.

  7. Immediate screening of lead exposure in the workplace using portable X-ray fluorescence.

    PubMed

    Gorce, Jean-Philippe; Roff, Martin

    2016-01-01

    The use of a portable X-ray fluorescence spectrometer (PXRF) equipped with a miniaturised X-ray tube producing a small 8 mm diameter X-ray beam required the validation of two new sampling protocols for the immediate screening of occupational lead exposure. First, lead in dust and fumes, collected by Institute of Occupational Medicine (IOM) inhalable samplers on 25 mm diameter membrane filters, is quantified using PXRF. To account for irregular dust deposition, the filters are rotated manually by quarter turns. Multiple PXRF readings are collected from the central region and from two locations in the outer region. The inner region is distinguishable from the outer region, but the two outer region locations are indistinguishable. High correlations (R(2) > 0.99) are found between the PXRF results and historical results obtained using a reference method based on a laboratory wavelength-dispersive sequential XRF instrument (WDXRF) for lead loadings between 1-161 μg. The PXRF results from the outer regions of the filters show a bias of -13% with respect to the WDXRF. Once this bias is allowed for, 95% of all PXRF results lie within -28% and +38% of the WDXRF results. Neither instrument accounts for potential dust accumulation on the walls of the IOM sampler. Therefore, methods based on their use can only be considered semi-quantitative. Second, a protocol combining direct PXRF measurements on workplace surfaces with surface wipes is designed for immediate on-site quantification of removable surface lead residues. The quantification of such residues by this method is compared with subsequent off-site wet chemistry analysis of the surface wipes. The two methods show a good correlation (R(2) ∼ 0.88). The ratio of the amount of removable residues determined by PXRF and wipe sampling is close to one with range 0.26-3.94. It is demonstrated that PXRF can be used as an effective tool for the immediate screening of occupational lead exposure. Although this article focused on

  8. Immediate screening of lead exposure in the workplace using portable X-ray fluorescence

    PubMed Central

    Gorce, Jean-Philippe; Roff, Martin

    2016-01-01

    ABSTRACT The use of a portable X-ray fluorescence spectrometer (PXRF) equipped with a miniaturised X-ray tube producing a small 8 mm diameter X-ray beam required the validation of two new sampling protocols for the immediate screening of occupational lead exposure. First, lead in dust and fumes, collected by Institute of Occupational Medicine (IOM) inhalable samplers on 25 mm diameter membrane filters, is quantified using PXRF. To account for irregular dust deposition, the filters are rotated manually by quarter turns. Multiple PXRF readings are collected from the central region and from two locations in the outer region. The inner region is distinguishable from the outer region, but the two outer region locations are indistinguishable. High correlations (R2 > 0.99) are found between the PXRF results and historical results obtained using a reference method based on a laboratory wavelength-dispersive sequential XRF instrument (WDXRF) for lead loadings between 1–161 μg. The PXRF results from the outer regions of the filters show a bias of −13% with respect to the WDXRF. Once this bias is allowed for, 95% of all PXRF results lie within −28% and +38% of the WDXRF results. Neither instrument accounts for potential dust accumulation on the walls of the IOM sampler. Therefore, methods based on their use can only be considered semi-quantitative. Second, a protocol combining direct PXRF measurements on workplace surfaces with surface wipes is designed for immediate on-site quantification of removable surface lead residues. The quantification of such residues by this method is compared with subsequent off-site wet chemistry analysis of the surface wipes. The two methods show a good correlation (R2 ∼ 0.88). The ratio of the amount of removable residues determined by PXRF and wipe sampling is close to one with range 0.26–3.94. It is demonstrated that PXRF can be used as an effective tool for the immediate screening of occupational lead exposure. Although this

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

    SciTech Connect

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

    2013-06-01

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

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

    PubMed

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

    2013-02-01

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

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

    PubMed

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

    2016-07-01

    Wilson's disease (WD) is a rare autosomal recessive disease due to mutations of the gene encoding the copper-transporter ATP7B. The diagnosis is hampered by the variability of symptoms induced by copper accumulation, the inconstancy of the pathognomonic signs and the absence of a reliable diagnostic test. We investigated the diagnostic potential of X-ray fluorescence (XRF) that allows quantitative analysis of multiple elements. Studies were performed on animal models using Wistar rats (n = 10) and Long Evans Cinnamon (LEC) rats (n = 11), and on human samples including normal livers (n = 10), alcohol cirrhosis (n = 8), haemochromatosis (n = 10), cholestasis (n = 6) and WD (n = 22). XRF experiments were first performed using synchrotron radiation to address the elemental composition at the cellular level. High-resolution mapping of tissue sections allowed measurement of the intensity and the distribution of copper, iron and zinc while preserving the morphology. Investigations were further conducted using a laboratory X-ray source for irradiating whole pieces of tissue. The sensitivity of XRF was highlighted by the discrimination of LEC rats from wild type even under a regimen using copper deficient food. XRF on whole formalin-fixed paraffin embedded needle biopsies allowed profiling of the elements in a few minutes. The intensity of copper related to iron and zinc significantly discriminated WD from other genetic or chronic liver diseases with 97.6% specificity and 100% sensitivity. This study established a definite diagnosis of Wilson's disease based on XRF. This rapid and versatile method can be easily implemented in a clinical setting. PMID:27499926

  12. Novel handheld x-ray fluorescence spectrometer for routine testing for the presence of lead

    NASA Astrophysics Data System (ADS)

    Rensing, Noa M.; Tiernan, Timothy C.; Squillante, Michael R.

    2011-06-01

    RMD is developing a safe, inexpensive, and easy to operate lead detector for retailers and consumers that can reliably detect dangerous levels of lead in toys and other household products. Lead and its compounds have been rated as top chemicals that pose a great threat to human health. However, widespread testing for environmental lead is rarely undertaken until lead poisoning has already been diagnosed. The problem is not due to the accuracy or sensitivity of existing lead detection technology, but rather to the high expense, safety and licensing barriers of available test equipment. An inexpensive and easy to use lead detector would enable the identification of highly contaminated objects and areas and allow for timely and cost effective remediation. The military has similar needs for testing for lead and other heavy elements such as mercury, primarily in the decontamination of former military properties prior to their return to civilian use. RMD's research and development efforts are abased on advanced solid-state detectors combined with recently patented lead detection techniques to develop a consumer oriented lead detector that will be widely available and easy and inexpensive to use. These efforts will result in an instrument that offers: (1) high sensitivity, to identify objects containing dangerous amounts of lead, (2) low cost to encourage widespread testing by consumers and other end users and (3) convenient operation requiring no training or licensing. In contrast, current handheld x-ray fluorescence spectrometers either use a radioactive source requiring licensing and operating training, or use an electronic x-ray source that limits their sensitivity to surface lead.

  13. Hard X-ray Fluorescence Measurements of Heteroepitaxial Solid Oxide Fuel Cell Cathode Materials

    SciTech Connect

    Davis, Jacob N.; Miara, Lincoln J.; Saraf, Laxmikant V.; Kaspar, Tiffany C.; Gopalan, Srikanth; Pal, Uday B.; Woicik, Joseph C.; Basu, Soumendra N.; Ludwig, Karl F.

    2012-12-01

    Commonly, SOFCs are operated at high temperatures (above 800°C). At these temperatures expensive housing is needed to contain an operating stack as well as coatings to contain the oxidation of the metallic interconnects. Lowering the temperature of an operating device would allow for more conventional materials to be used, thus lowering overall cost. Understanding the surface chemical states of cations in the surface of the SOFC cathode is vital to designing a system that will perform well at lower temperatures. The samples studied were grown by pulsed laser deposition (PLD) at the Environmental Molecular Sciences Laboratory (EMSL) at Pacific Northwest National Laboratory (PNNL). 20% strontium doped lanthanum manganite (LSM-20) was grown on YSZ and NGO (neodymium gallate). The films on YSZ have a fiber texture. LSM-20 on NGO is heteroepitaxial. Lanthanum strontium cobalt ferrite (LSCF-6428) films were grown on LAO and YSZ with a GDC barrier layer. Total X-ray Reflection Fluorescence (TXRF) was used to depth profile the samples. In a typical experiment, the angle of the incident beam is varied though the critical angle. Below the critical angle, the x-ray decays as an evanescent wave and will only penetrate the top few nanometers. TXRF experiments done on LSM films have suggested strontium segregates to the surface and form strontium enriched nanoparticles (1). It should be pointed out that past studies have focused on 30% strontium A-site doping, but this project uses 20% strontium doped lanthanum manganite. XANES and EXAFS data were taken as a function of incoming angle to probe composition as a function of depth. XANES spectra can be difficult to analyze fully. For other materials density functional theory calculations compared to near edge measurements have been a good way to understand the 3d valence electrons (2).

  14. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates

    DOE PAGESBeta

    Huang, H. Y.; Jia, C. J.; Chen, Z. Y.; Wohlfeld, K.; Moritz, B.; Devereaux, T. P.; Wu, W. B.; Okamoto, J.; Lee, W. S.; Hashimoto, M.; et al

    2016-01-22

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O8+δ. Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast,more » the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors.« less

  15. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates

    PubMed Central

    Huang, H. Y.; Jia, C. J.; Chen, Z. Y.; Wohlfeld, K.; Moritz, B.; Devereaux, T. P.; Wu, W. B.; Okamoto, J.; Lee, W. S.; Hashimoto, M.; He, Y.; Shen, Z. X.; Yoshida, Y.; Eisaki, H.; Mou, C. Y.; Chen, C. T.; Huang, D. J.

    2016-01-01

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O8+δ. Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast, the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors. PMID:26794437

  16. Improved micro x-ray fluorescence spectrometer for light element analysis

    SciTech Connect

    Smolek, Stephan; Streli, Christina; Zoeger, Norbert; Wobrauschek, Peter

    2010-05-15

    Since most available micro x-ray fluorescence (micro-XRF) spectrometers operate in air, which does not allow the analysis of low-Z elements (Z{<=}14), a special micro-XRF spectrometer has been designed to extend the analytical range down to light elements (Z{>=}6). It offers improved excitation and detection conditions necessary for light element analysis. To eliminate absorption of the exciting and fluorescent radiation, the system operates under vacuum condition. Sample mapping is automated and controlled by specialized computer software developed for this spectrometer. Several different samples were measured to test and characterize the spectrometer. The spot size has been determined by scans across a 10 {mu}m Cu wire which resulted in a full width at half maximum of 31 {mu}m for Mo K{alpha} line (17.44 keV) and 44 {mu}m effective beam size for the Cu K edge and 71 {mu}m effective beam size for the Cu L edge. Lower limits of detection in the picogram range for each spot (or {mu}g/cm{sup 2}) were obtained by measuring various thin metal foils under different conditions. Furthermore, detection limits in the parts per million range were found measuring NIST621 standard reference material. Area scans of a microscopic laser print and NaF droplet were performed to show mapping capabilities.

  17. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates

    NASA Astrophysics Data System (ADS)

    Huang, H. Y.; Jia, C. J.; Chen, Z. Y.; Wohlfeld, K.; Moritz, B.; Devereaux, T. P.; Wu, W. B.; Okamoto, J.; Lee, W. S.; Hashimoto, M.; He, Y.; Shen, Z. X.; Yoshida, Y.; Eisaki, H.; Mou, C. Y.; Chen, C. T.; Huang, D. J.

    2016-01-01

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O8+δ. Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast, the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors.

  18. Raman and fluorescence characteristics of resonant inelastic X-ray scattering from doped superconducting cuprates.

    PubMed

    Huang, H Y; Jia, C J; Chen, Z Y; Wohlfeld, K; Moritz, B; Devereaux, T P; Wu, W B; Okamoto, J; Lee, W S; Hashimoto, M; He, Y; Shen, Z X; Yoshida, Y; Eisaki, H; Mou, C Y; Chen, C T; Huang, D J

    2016-01-01

    Measurements of spin excitations are essential for an understanding of spin-mediated pairing for superconductivity; and resonant inelastic X-ray scattering (RIXS) provides a considerable opportunity to probe high-energy spin excitations. However, whether RIXS correctly measures the collective spin excitations of doped superconducting cuprates remains under debate. Here we demonstrate distinct Raman- and fluorescence-like RIXS excitations of Bi1.5Pb0.6Sr1.54CaCu2O(8+δ). Combining photon-energy and momentum dependent RIXS measurements with theoretical calculations using exact diagonalization provides conclusive evidence that the Raman-like RIXS excitations correspond to collective spin excitations, which are magnons in the undoped Mott insulators and evolve into paramagnons in doped superconducting compounds. In contrast, the fluorescence-like shifts are due primarily to the continuum of particle-hole excitations in the charge channel. Our results show that under the proper experimental conditions RIXS indeed can be used to probe paramagnons in doped high-Tc cuprate superconductors. PMID:26794437

  19. Multispectral processing of combined visible and x-ray fluorescence imagery in the Archimedes palimpsest

    NASA Astrophysics Data System (ADS)

    Walvoord, Derek; Bright, Allison; Easton, Roger L., Jr.

    2008-02-01

    The Archimedes palimpsest is one of the most significant early texts in the history of science that has survived to the present day. It includes the oldest known copies of text from seven treatises by Archimedes, along with pages from other important historical writings. In the 13th century, the original texts were erased and overwritten by a Christian prayer book, which was used in religious services probably into the 19th century. Since 2001, much of the text from treatises of Archimedes has been transcribed from images taken in reflected visible light and visible fluorescence generated by exposure of the parchment to ultraviolet light. However, these techniques do not work well on all pages of the manuscript, including the badly stained colophon, four pages of the manuscript obscured by icons painted during the first half of the 20th century, and some pages of non-Archimedes texts. Much of the text on the colophon and overpainted pages has been recovered from X-ray fluorescence (XRF) imagery. In this work, the XRF images of one of the other pages were combined with the bands of optical images to create hyperspectral image cubes and processed using standard statistical classification techniques developed for environmental remote sensing to test if this improved the recovery of the original text.

  20. ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT - FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER - METOREX, INC. X-MET 920-P AND 940

    EPA Science Inventory

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

  1. FIELD MEASUREMENT TECHNOLOGY FOR MERCURY IN SOIL AND SEDIMENT NITON'S XLI/XLT 700 SERIES X-RAY FLUORESCENCE ANALYZER

    EPA Science Inventory

    NITON's XL-700 Series X-ray fluorescence analyzers were demonstrated under the U.S. Environmental Protection Agency Superfund Innovative Technology Evaluation Program in May 2003 at the Oak Ridge National Laboratory (ORNL) in Oak Ridge, Tennessee. The purpose of the Demonstration...

  2. EVALUATION OF PORTABLE X-RAY FLUORESCENCE SPECTROMETER FOR MEASUREMENT OF LEAD IN PAINT, SOIL AND DUST

    EPA Science Inventory

    Three widely used commercially available portable X-ray fluorescence spectrometers were evaluated for precision and accuracy of measurement of lead in paint. ncluded were two direct reading instruments and one spectrum analyzer. est materials were prepared by spiking oil-based an...

  3. ENERGY DISPERSIVE X-RAY FLUORESCENCE ANALYSIS OF DUST COLLECTED USING A VERTICAL ELUTRIATOR COTTON DUST SAMPLER

    EPA Science Inventory

    X-ray fluorescence (XRF) spectroscopy has been used to analyze trace element concentrations in cotton dusts collected on verticle elutriator filter media. Twenty-three samples collected from ten bales of cotton processed in a model card room have been analyzed. The major elements...

  4. Log spiral of revolution highly oriented pyrolytic graphite monochromator for fluorescence x-ray absorption edge fine structure

    SciTech Connect

    Pease, D. M.; Daniel, M.; Budnick, J. I.; Rhodes, T.; Hammes, M.; Potrepka, D. M.; Sills, K.; Nelson, C.; Heald, S. M.; Brewe, D. I.

    2000-09-01

    We have constructed an x-ray monochromator based on a log spiral of revolution covered with highly oriented pyrolytic graphite. Such a monochromator is used for obtaining x-ray absorption edge fine structure by the fluorescence method, and is particularly useful for measuring the fine structure of dilute element A in a concentrated matrix of element B, where B is to the left of A in the Periodic Table. Using the log spiral monochromator, we measure good Cr x-ray fine structure in an alloy of 1% Cr in a V matrix, whereas the corresponding spectrum is severely distorted by the V background if nonmonochromatized fluorescence is used. We also obtain excellent rejection of Mn fluorescence relative to Cr fluorescence in a Cr{sub 80}Mn{sub 20} alloy, and can tune the monochromator such that the entire Mn step height is significantly smaller than the Cr x-ray absorption edge fine structure oscillations for this system. (c) 2000 American Institute of Physics.

  5. VERIFICATION OF A PARTICLE SIZE CORRECTION METHOD FOR X-RAY FLUORESCENCE SPECTROMETRIC ANALYSIS OF ENVIRONMENTAL SAMPLES

    EPA Science Inventory

    Platinum tetraiodide aerosols generated with a spinning disk from solutions in ethanol were used to test a particle size correction factor recently proposed by Criss for the X-ray fluorescence analysis of filter-deposited particulate samples. A set of standards of well-defined pa...

  6. [Influence of the Experiment Energy Dispersive X-Ray Fluorescence Measurement of Uranium by Different Excitation Source].

    PubMed

    Xiong, Chao; Ge, Liang-quan; Liu, Duan; Zhang, Qing-xian; Gu, Yi; Luo, Yao-yao; Zhao, Jian-kun

    2016-03-01

    Aiming at the self-excitation effect on the interference of measurements which exist in the process of Energy dispersive X-ray fluorescence method for uranium measurement. To solve the problem of radioactive isotopes only used as excitation source in determination of uranium. Utilizing the micro X-ray tube to test Self-excitation effect to get a comparison of the results obtained by three different uranium ore samples--109 Cd, 241 Am and Mirco X-ray tube. The results showed that self-excitation effect produced the area measure of characteristic X-ray peak is less than 1% of active condition, also the interference of measurements can be negligible. Photoelectric effect cross-section excited by 109 Cd is higher, corresponding fluorescence yield is higher than excited by 241 Am as well due to characteristics X-ray energy of 109 Cd, 22.11 & 24.95 KeV adjacent to absorption edge energy of L(α), 21.75 KeV, based on the above, excitation efficiency by 109 Cd is higher than 241 Am; The fact that measurement error excited by 241 Am is significantly greater than by 109 Cd is mainly due to peak region overlap between L energy peaks of uranium and Scattering peak of 241 Am, 26.35 keV, These factors above caused the background of measured Spectrum higher; The error between the uranium content in ore samples which the X-ray tube as the excitation source and the chemical analysis results is within 10%. Conclusion: This paper come to the conclusion that the technical quality of uranium measurement used X-ray tube as excitation source is superior to that in radioactive source excitation mode. PMID:27400534

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

    SciTech Connect

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

    2009-12-15

    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.

  8. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis

    DOE PAGESBeta

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Ward, Jesse; Deng, Junjing; Mak, Rachel; Moonier, Nena; et al

    2015-02-23

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologicallymore » important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results.« less

  9. Fast-scanning high-flux microprobe for biological X-ray fluorescence microscopy and microXAS

    SciTech Connect

    Barrea, R.A.; Gore, D.; Kujala, N.; Karanfil, C.; Kozyrenko, S.; Heurich, R.; Vukonich, M.; Huang, R.; Paunesku, T.; Woloschak, G.; Irving, T.C.

    2010-07-23

    There is a growing interest in the biomedical community in obtaining information concerning the distribution and local chemical environment of metals in tissues and cells. Recently, biological X-ray fluorescence microscopy (XFM) has emerged as the tool of choice to address these questions. A fast-scanning high-flux X-ray microprobe, built around a recently commissioned pair of 200 mm-long Rh-coated silicon Kirkpatrick-Baez mirrors, has been constructed at BioCAT beamline 18ID at the Advanced Photon Source. The new optical system delivers a flux of 1.3 x 10{sup 12} photons s{sup -1} into a minimum focal spot size of {approx}3-5 {micro}m FWHM. A set of Si drift detectors and bent Laue crystal analyzers may be used in combination with standard ionization chambers for X-ray fluorescence measurements. BioCAT's scanning software allows fast continuous scans to be performed while acquiring and storing full multichannel analyzer spectra per pixel on-the-fly with minimal overhead time (<20 ms per pixel). Together, the high-flux X-ray microbeam and the rapid-scanning capabilities of the BioCAT beamline allow the collection of XFM and micro X-ray absorption spectroscopy (microXAS) measurements from as many as 48 tissue sections per day. This paper reports the commissioning results of the new instrument with representative XFM and microXAS results from tissue samples.

  10. Fast-scanning high-flux microprobe for biological X-ray fluorescence microscopy and microXAS.

    PubMed

    Barrea, R A; Gore, D; Kujala, N; Karanfil, C; Kozyrenko, S; Heurich, R; Vukonich, M; Huang, R; Paunesku, T; Woloschak, G; Irving, T C

    2010-07-01

    There is a growing interest in the biomedical community in obtaining information concerning the distribution and local chemical environment of metals in tissues and cells. Recently, biological X-ray fluorescence microscopy (XFM) has emerged as the tool of choice to address these questions. A fast-scanning high-flux X-ray microprobe, built around a recently commissioned pair of 200 mm-long Rh-coated silicon Kirkpatrick-Baez mirrors, has been constructed at BioCAT beamline 18ID at the Advanced Photon Source. The new optical system delivers a flux of 1.3 x 10(12) photons s(-1) into a minimum focal spot size of approximately 3-5 microm FWHM. A set of Si drift detectors and bent Laue crystal analyzers may be used in combination with standard ionization chambers for X-ray fluorescence measurements. BioCAT's scanning software allows fast continuous scans to be performed while acquiring and storing full multichannel analyzer spectra per pixel on-the-fly with minimal overhead time (<20 ms per pixel). Together, the high-flux X-ray microbeam and the rapid-scanning capabilities of the BioCAT beamline allow the collection of XFM and micro X-ray absorption spectroscopy (microXAS) measurements from as many as 48 tissue sections per day. This paper reports the commissioning results of the new instrument with representative XFM and microXAS results from tissue samples. PMID:20567085

  11. Quantitative imaging of gold nanoparticle distribution in a tumor-bearing mouse using benchtop x-ray fluorescence computed tomography

    PubMed Central

    Manohar, Nivedh; Reynoso, Francisco J.; Diagaradjane, Parmeswaran; Krishnan, Sunil; Cho, Sang Hyun

    2016-01-01

    X-ray fluorescence computed tomography (XFCT) is a technique that can identify, quantify, and locate elements within objects by detecting x-ray fluorescence (characteristic x-rays) stimulated by an excitation source, typically derived from a synchrotron. However, the use of a synchrotron limits practicality and accessibility of XFCT for routine biomedical imaging applications. Therefore, we have developed the ability to perform XFCT on a benchtop setting with ordinary polychromatic x-ray sources. Here, we report our postmortem study that demonstrates the use of benchtop XFCT to accurately image the distribution of gold nanoparticles (GNPs) injected into a tumor-bearing mouse. The distribution of GNPs as determined by benchtop XFCT was validated using inductively coupled plasma mass spectrometry. This investigation shows drastically enhanced sensitivity and specificity of GNP detection and quantification with benchtop XFCT, up to two orders of magnitude better than conventional x-ray CT. The results also reaffirm the unique capabilities of benchtop XFCT for simultaneous determination of the spatial distribution and concentration of nonradioactive metallic probes, such as GNPs, within the context of small animal imaging. Overall, this investigation identifies a clear path toward in vivo molecular imaging using benchtop XFCT techniques in conjunction with GNPs and other metallic probes. PMID:26912068

  12. Quantitative imaging of gold nanoparticle distribution in a tumor-bearing mouse using benchtop x-ray fluorescence computed tomography

    NASA Astrophysics Data System (ADS)

    Manohar, Nivedh; Reynoso, Francisco J.; Diagaradjane, Parmeswaran; Krishnan, Sunil; Cho, Sang Hyun

    2016-02-01

    X-ray fluorescence computed tomography (XFCT) is a technique that can identify, quantify, and locate elements within objects by detecting x-ray fluorescence (characteristic x-rays) stimulated by an excitation source, typically derived from a synchrotron. However, the use of a synchrotron limits practicality and accessibility of XFCT for routine biomedical imaging applications. Therefore, we have developed the ability to perform XFCT on a benchtop setting with ordinary polychromatic x-ray sources. Here, we report our postmortem study that demonstrates the use of benchtop XFCT to accurately image the distribution of gold nanoparticles (GNPs) injected into a tumor-bearing mouse. The distribution of GNPs as determined by benchtop XFCT was validated using inductively coupled plasma mass spectrometry. This investigation shows drastically enhanced sensitivity and specificity of GNP detection and quantification with benchtop XFCT, up to two orders of magnitude better than conventional x-ray CT. The results also reaffirm the unique capabilities of benchtop XFCT for simultaneous determination of the spatial distribution and concentration of nonradioactive metallic probes, such as GNPs, within the context of small animal imaging. Overall, this investigation identifies a clear path toward in vivo molecular imaging using benchtop XFCT techniques in conjunction with GNPs and other metallic probes.

  13. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis

    SciTech Connect

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Ward, Jesse; Deng, Junjing; Mak, Rachel; Moonier, Nena; Jacobsen, Chris; Brody, James P.

    2015-02-23

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologically important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results.

  14. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis.

    PubMed

    Jin, Qiaoling; Vogt, Stefan; Lai, Barry; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Ward, Jesse; Deng, Junjing; Mak, Rachel; Moonier, Nena; Jacobsen, Chris

    2015-01-01

    Rapidly-frozen hydrated (cryopreserved) specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologically important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results. PMID:25706293

  15. Quantitative imaging of gold nanoparticle distribution in a tumor-bearing mouse using benchtop x-ray fluorescence computed tomography.

    PubMed

    Manohar, Nivedh; Reynoso, Francisco J; Diagaradjane, Parmeswaran; Krishnan, Sunil; Cho, Sang Hyun

    2016-01-01

    X-ray fluorescence computed tomography (XFCT) is a technique that can identify, quantify, and locate elements within objects by detecting x-ray fluorescence (characteristic x-rays) stimulated by an excitation source, typically derived from a synchrotron. However, the use of a synchrotron limits practicality and accessibility of XFCT for routine biomedical imaging applications. Therefore, we have developed the ability to perform XFCT on a benchtop setting with ordinary polychromatic x-ray sources. Here, we report our postmortem study that demonstrates the use of benchtop XFCT to accurately image the distribution of gold nanoparticles (GNPs) injected into a tumor-bearing mouse. The distribution of GNPs as determined by benchtop XFCT was validated using inductively coupled plasma mass spectrometry. This investigation shows drastically enhanced sensitivity and specificity of GNP detection and quantification with benchtop XFCT, up to two orders of magnitude better than conventional x-ray CT. The results also reaffirm the unique capabilities of benchtop XFCT for simultaneous determination of the spatial distribution and concentration of nonradioactive metallic probes, such as GNPs, within the context of small animal imaging. Overall, this investigation identifies a clear path toward in vivo molecular imaging using benchtop XFCT techniques in conjunction with GNPs and other metallic probes. PMID:26912068

  16. Fast-scanning high-flux microprobe for biological X-ray fluorescence microscopy and microXAS

    PubMed Central

    Barrea, R. A.; Gore, D.; Kujala, N.; Karanfil, C.; Kozyrenko, S.; Heurich, R.; Vukonich, M.; Huang, R.; Paunesku, T.; Woloschak, G.; Irving, T. C.

    2010-01-01

    There is a growing interest in the biomedical community in obtaining information concerning the distribution and local chemical environment of metals in tissues and cells. Recently, biological X-ray fluorescence microscopy (XFM) has emerged as the tool of choice to address these questions. A fast-scanning high-flux X-ray microprobe, built around a recently commissioned pair of 200 mm-long Rh-coated silicon Kirkpatrick–Baez mirrors, has been constructed at BioCAT beamline 18ID at the Advanced Photon Source. The new optical system delivers a flux of 1.3 × 1012 photons s−1 into a minimum focal spot size of ∼3–5 µm FWHM. A set of Si drift detectors and bent Laue crystal analyzers may be used in combination with standard ionization chambers for X-ray fluorescence measurements. BioCAT’s scanning software allows fast continuous scans to be performed while acquiring and storing full multichannel analyzer spectra per pixel on-the-fly with minimal overhead time (<20 ms per pixel). Together, the high-flux X-ray microbeam and the rapid-scanning capabilities of the BioCAT beamline allow the collection of XFM and micro X-ray absorption spectroscopy (microXAS) measurements from as many as 48 tissue sections per day. This paper reports the commissioning results of the new instrument with representative XFM and microXAS results from tissue samples. PMID:20567085

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

    SciTech Connect

    Carlisle, J.A.; Shirley, E.L.; Hudson, E.A.

    1997-04-01

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

  18. Fingerprint methods for suspended sediment transport processes by using X-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Nakayama, K.; Beitia, C.; Ohtsu, N.; Yamasaki, S.; Yasuyuki, M.; Yamane, M.

    2014-12-01

    Suspended sediment (SS) can have significant impacts on ecological system, and high SS concentration can have significant impacts on human life. In the previous studies, radionuclide analysis has been applied to evaluate the production of SS in the river basins, which demonstrated that the surface soil erosion can be estimated by using radionuclide Pb-210ex. However, radionuclide analysis cannot indicate the relative amounts of SS transported from each individual sub-basin to the downstream end. Thus, X-ray Fluorescence Analysis (XRF Analysis) can be considered as an alternative method to radionuclide analysis because the XRF Analysis can measure 21 chemical compositions, Na2O, MgO, Al2O3, SiO2, P2O5, SO3, Cl, K2O, CaO, TiO2, Cr2O3, MnO, Fe2O3, Co2O3, NiO, CuO, ZnO, Rb2O, SrO, BaO, and Y2O3 by using X-ray Fluorescence Analyzer. In June of 2007, high turbidity, which is more than 10,000 (NTU), was measured in the Oromushi River basin of Hokkaido in Japan. Therefore, this study aims to clarify the mechanism of the transport of SS in the Oromushi River basin. We measured chemical compositions of soil with diameter less than 63 μm in the Oromushi River basin in order to pay attention to SS by using XRF. The Principal Component Analysis revealed that SiO2, Al2O3, Fe2O3, CaO and Na2O are the dominant chemical compositions. Although the predominant composition was the same in a river basin including the downstream end, significant differences were found in the pattern of chemical compositions. Therefore, by using the chemical compositions of SiO2, Al2O3, Fe2O3, CaO and Na2O, the Mixing Stable Isotope Analysis in R model (MixSIAR) based on Bayesian statistics was applied to estimate the transportation rate of SS from each sub-basin to the downstream end, which agreed with the field experiment results very well. As a result, spatial patterns of SS transportation rate are found to be strongly related to surface soil type.

  19. Gemas: issues from the comparison of aqua regia and X-ray fluorescence results

    NASA Astrophysics Data System (ADS)

    Dinelli, Enrico; Birke, Manfred; Reimann, Clemens; Demetriades, Alecos; DeVivo, Benedetto; Flight, Dee; Ladenberger, Anna; Albanese, Stefano; Cicchella, Domenico; Lima, Annamaria

    2014-05-01

    The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution in soil. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database, consisting of 2 x ca. 2100 samples spread evenly over 33 European countries, is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the Geological Survey of the Slovak Republic, AR analyses were carried out at ACME Labs, and XRF analyses at the Federal Institute for Geosciences and Natural Resources, Germany Element recovery by AR is very different, ranging from <1% (e.g. Na, Zr) to > 80% (e.g. Mn, P, Co). Recovery is controlled by mineralogy of the parent material, but geographic and climatic factors and the weathering history of the soils are also important. Nonetheless, even the very low recovery elements show wide ranges of variation and spatial patterns that are affected by other factors than soil parent material. For many elements soil pH have a clear influence on AR extractability: under acidic soil conditions almost all elements tend to be leached and their extractability is generally low. It progressively increases with increasing pH and is highest in the pH range 7-8. Critical is the clay content of the soil

  20. Watershed-Scale Geochemical Inventory of Soils by Portable X-Ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Beaudette, D. E.; Stupi, L. K.; Swarowsky, A.; O'Geen, A. T.; Chang, J. F.; Gallagher, B.

    2009-12-01

    Spatial databases of geochemical data are an excellent source of point-scale information on naturally occurring toxic elements (arsenic, selenium or radon), contamination from industrial processes (lead, mercury, or cesium), mineralogical variability, and the fate of toxic compounds (i.e. sorption of pesticides to iron oxyhydroxide minerals) in soil. Sample preparation time, safety concerns associated with HF or HNO3 acid dissolution, instrument availability, and cost are all common constraints that limit the scale at which new geochemical surveys can be conducted. We used a Thermo-Fisher Niton portable X-Ray fluorescence (XRF) meter to perform comparatively rapid geochemical surveys in soils of two (35 ha) watersheds. The watersheds have contrasting parent materials, one formed from metavolcanic rock and the other from granite. The X-Ray fluorescence inventory of genetic soil horizons (n=660) was used to identify trends in soil development and landscape processes. Since soil samples are usually sieved and ground for standard laboratory characterization, the additional time required to prepare samples for XRF analysis was minimal, approximately 2 minutes for sample preparation and 6 minutes for machine scan time per sample. Preliminary analysis of the resulting geochemical data show strong spatial trends in watershed- and hillslope-scale variability in weathering indices (FeCBD:FeTotal and K:Ti), inferred mineralogy (Si:Al, Si:Al+Fe), and geologic signatures (multivariate analysis of 20 common elements). Depth trends and spatial patterns were correlated with common terrain-shape indices (slope, upslope contributing area, surface curvatures, local prominence, etc.), degree of soil development, parent material, and hydrological conditions. For example, Si:Al was higher in soils with greater upslope contributing area, and in seasonally saturated soils (Fig 1). Our findings demonstrate that portable XRF technology is a promising new tool for rapid lab-based and in situ

  1. Synchrotron x-ray fluorescence microprobe: Quantification and mapping of mixed valence state samples using micro-XANES

    SciTech Connect

    Sutton, S.R. ); Bajt, S. Department of Applied Science, Brookhaven National Laboratory, Upton, New York 11973 ); Delaney, J. ); Schulze, D. ); Tokunaga, T. )

    1995-02-01

    The synchrotron x-ray fluorescence microprobe is a valuable instrument for quantification and mapping of mixed valence state samples with high spatial resolution and elemental sensitivity. A method has been developed for quantifying the proportions of Fe[sup 2+] and Fe[sup 3+] with 100 [mu]m spatial resolution and better than 100 ppm sensitivity using x-ray absorption near-edge structure (XANES). Applications of valence state mapping have been made to selenium in water-saturated sediments and manganese associated with wheat roots attacked by the take-all fungus.

  2. Analytic 3D Imaging of Mammalian Nucleus at Nanoscale Using Coherent X-Rays and Optical Fluorescence Microscopy

    PubMed Central

    Song, Changyong; Takagi, Masatoshi; Park, Jaehyun; Xu, Rui; Gallagher-Jones, Marcus; Imamoto, Naoko; Ishikawa, Tetsuya

    2014-01-01

    Despite the notable progress that has been made with nano-bio imaging probes, quantitative nanoscale imaging of multistructured specimens such as mammalian cells remains challenging due to their inherent structural complexity. Here, we successfully performed three-dimensional (3D) imaging of mammalian nuclei by combining coherent x-ray diffraction microscopy, explicitly visualizing nuclear substructures at several tens of nanometer resolution, and optical fluorescence microscopy, cross confirming the substructures with immunostaining. This demonstrates the successful application of coherent x-rays to obtain the 3D ultrastructure of mammalian nuclei and establishes a solid route to nanoscale imaging of complex specimens. PMID:25185543

  3. Photospheric Fluorescence and Resonance Scattering: Non Classical Diagnostics and the Future of X-ray Stellar Spectroscopy

    NASA Technical Reports Server (NTRS)

    Drake, Jeremy

    1998-01-01

    High resolution AXAF and XMM observations of stellar coronae will yield a wealth of X-ray plasma line diagnostics that will provide a giant leap forward in our understanding of coronal densities, abundance anomalies and emission measure distributions. Unfortunately, there is one very basic unanswered question in the physics of active stellar coronae that the usual plasma diagnostics cannot address directly: What are the spatial characteristics of stellar coronae-the scale height and filling factor? What do other stellar coronae actually look like? I will discuss two novel diagnostics of coronal geometry and their application to future X-ray spectra: photospheric fluorescence and resonance line optical depths.

  4. Optimization of sample preparation for grazing emission X-ray fluorescence in micro- and trace analysis applications

    NASA Astrophysics Data System (ADS)

    Claes, Martine; de Bokx, Pieter; Willard, Nico; Veny, Paul; Van Grieken, René

    1997-07-01

    Grazing emission X-ray fluorescence (GEXRF) is a new development in X-ray fluorescence analysis related to total-reflection XRF. An optical flat carrying the sample is irradiated at an angle of approximately 90° with an uncollimated polychromatic X-ray beam. The emitted fluorescent radiation of the sample elements is measured at very small angles using wavelength dispersive detection. For the application of GEXRF in micro- and trace analysis, a sample preparation procedure for analysis of liquid samples has been developed. Polycarbonate was investigated as a possible material for the sample carrier. Homogeneous distribution of the sample on the support was achieved by special pre-treatment of the carrier. This pre-treatment includes siliconizing the polycarbonate disks with Serva silicone solution, after which the siliconized carriers are placed in an oxygen plasma asher. Finally, to obtain a spot of the same size as the X-ray beam (≈30 mm diameter), a thin silicone layer is placed as a ring on the carriers with an ear pick. Electron microprobe analyses were performed to check the distribution of the liquid sample deposit, and GEXRF measurements were used to check the reproducibility of sample preparation.

  5. [Research on the X-ray fluorescence spectrometry method to determine trace elements in kimberlite].

    PubMed

    Zhang, Lei; Yan, Chuan-wei; Lu, Yi

    2003-04-01

    It is very important to detect trace elements for kilmberlite. Through improving the working conditions of X-ray fluorescence spectrometer and optimizing the analytical conditions, the determination method of trace elements, such as Sc, Cr, Ni, Y, Nb, La, in kimberlite was worked out. The method has been successfully applied to the determination of trace elements in over 2 thousand samples of kimberlite from Liaoning province. The detection limits of the method were relatively low (the detection limit of Sc droped from 9.54 to 2.83 micrograms.g-1 and the detection limit of La droped from 21.68 micrograms.g-1 to 9.18 micrograms.g-1), i.e. 2.83, 2.15, 2.20, 1.17, 1.05 and 9.18 micrograms.g-1 for Sc, Cr, Ni, Y, Nb and La, respectively. The precision of the method was very high with 2.10%-7.09% of RSD (n = 20). Compared with ICP spectrometry this method is satisfactory. The method has proven to be simple and rapid with low cost and high efficiency. PMID:12961906

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

    NASA Astrophysics Data System (ADS)

    Gonzalez-Fernandez, O.; Queralt, I.; Carvalho, M. L.; Garcia, G.

    2007-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

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

  8. Algorithms for a hand-held miniature x-ray fluorescence analytical instrument

    SciTech Connect

    Elam, W.T.; Newman, D.; Ziemba, F.

    1998-12-31

    The purpose of this joint program was to provide technical assistance with the development of a Miniature X-ray Fluorescence (XRF) Analytical Instrument. This new XRF instrument is designed to overcome the weaknesses of spectrometers commercially available at the present time. Currently available XRF spectrometers (for a complete list see reference 1) convert spectral information to sample composition using the influence coefficients technique or the fundamental parameters method. They require either a standard sample with composition relatively close to the unknown or a detailed knowledge of the sample matrix. They also require a highly-trained operator and the results often depend on the capabilities of the operator. In addition, almost all existing field-portable, hand-held instruments use radioactive sources for excitation. Regulatory limits on such sources restrict them such that they can only provide relatively weak excitation. This limits all current hand-held XRF instruments to poor detection limits and/or long data collection times, in addition to the licensing requirements and disposal problems for radioactive sources. The new XRF instrument was developed jointly by Quantrad Sensor, Inc., the Naval Research Laboratory (NRL), and the Department of Energy (DOE). This report describes the analysis algorithms developed by NRL for the new instrument and the software which embodies them.

  9. Environmental air degradation in Dar es Salaam by x-ray fluorescence.

    PubMed

    Koleleni, Y I A

    2002-03-01

    In Dar es Salaam a study of the aerosol contents was conducted and particulate matter on the filters were collected using an Andersen PM10 impactor to determine the environmental air pollution. The contents were determined by X-ray fluorescence analysis. In this study sources of environmental degradation and the concentrations were named as follows: Combustion processes with range of Br from 10 to 800 ng/m3, Pb from 30 to 790 ng/m3. Industrial processes with range of Fe from 37 to 883 ng/m3, Cu from 14 to 310 ng/m3, Zn from 6 to 820ng/m3. Top soil activities with range of K from 20 to 540 ng/m3, Ca from 24 to 3805 ng/m3, Ti from 2 to 59 ng/m3, Mn from 10 to 386 ng/m3. Marine processes with range of Cl from 20 to 310 ng/m3, S from 72 to 134 ng/m3. PMID:11930944

  10. Effects of overlying soft tissue on X-ray fluorescence bone lead measurement uncertainty

    NASA Astrophysics Data System (ADS)

    Ahmed, Naseer; Fleming, David E. B.; Wilkie, David; O'Meara, Joanne M.

    2006-01-01

    The effects of overlying soft tissue on the measurement uncertainty of the in vivo 109Cd K-shell X-ray fluorescence (XRF) technique were investigated, as applied to the tibia bone site. Experimental measurements were performed on a set of nine leg phantoms of different soft tissue thickness, intended to model the lower leg at mid-tibia. A standard bone phantom made from plaster-of-Paris and having a nominal lead concentration of 25.6 μg Pb per gram was used in all trials. Monte Carlo simulations of the experimental set-up were also performed. Results indicate a strong relation between measurement uncertainty and overlying tissue thickness (OTT) for the XRF bone lead method. In increasing the OTT from 3.2 to 14.6 mm, an increase in average measurement uncertainty by a factor of 2.40 was observed experimentally. Monte Carlo simulations indicated an increase in minimum detectable limit (MDL) by a factor of 2.46 over the same interval. Experimental and Monte Carlo results were generally in strong agreement. For subject screening purposes, direct measurement of soft tissue overlying the tibia is recommended whenever practical.

  11. Repeatability of tibia lead measurement by X-Ray fluorescence in a battery-making workforce.

    PubMed

    Todd, A C; Ehrlich, R I; Selby, P; Jordaan, E

    2000-11-01

    The purpose of this study was to remeasure in vivo tibia lead levels in a lead-acid battery manufacturing workforce measured in a previous survey and believed to be unrealistically high. Tibia lead levels were measured by K-shell X-ray fluorescence (XRF) spectroscopy in a stratified random sample (n=40) of the original study group (n=381). The repeat survey showed much lower tibia lead levels (median=54.3 microg lead/g bone mineral, compared to 217.9 microg lead/g bone mineral, n=40). Tibia lead levels were significantly correlated with duration of occupational exposure, zinc protoporphyrin levels, and cumulative blood lead index, but not with current blood lead levels. Thirty-eight of the 40 subjects underwent two consecutive tibia lead measurements to assess the test-retest repeatability of the XRF tibia lead measurement technique. The intraclass correlation coefficient between repeated measurements was 0.926 (P=0.0001). Three measurement pairs differed by more than 20 microg/g. There was no fixed or proportional bias between the two sets of measurements. We conclude that the technique offers a highly repeatable measurement of tibia bone lead. However, care needs to be taken to avoid contamination when performing measurements on active lead workers. PMID:11097802

  12. Optimal configuration for detection of gold nanoparticles in tumors using Kβ X-ray fluorescence line

    NASA Astrophysics Data System (ADS)

    Figueroa, R. G.; Santibañez, M.; Malano, F.; Valente, M.

    2015-12-01

    This study examines the increase in the capacity to detect gold nanoparticles in tumor tissue using X-rays from orthovoltage sources. The analyzed methodology considered aspects of geometry and composition in accordance with those required in real clinical treatment applications. The results show that a geometrical backscatter configuration, an incident spectral energy synthesized to optimize statistical parameters and adequate background subtraction allow for a significant increase in the signal to noise ratio (SNR) of the secondary Kβ lines. This increase is greater than those currently reported for traditional Kα lines. Furthermore, these conditions also produce an increase in detection sensitivity, less uncertainty in results and shorter exposure times. The proposed methodology was evaluated using XMI-MSIM software for the Monte Carlo simulation fluorescent response of each element. The simulation used tumors of 1-3 cm3, at a depth of 1-5 cm with a 0.1-1% gold nanoparticle concentration. The measurement time and the skin entrance dose by the methodology were considered for allows future quantitative surface scanning implementation.

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

    NASA Astrophysics Data System (ADS)

    Pessanha, Sofia; Madeira, Teresa I.; Manso, Marta; Guerra, Mauro; Le Gac, Agnès; Carvalho, Maria Luisa

    2014-09-01

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

  14. X-ray fluorescence spectroscopy and Monte Carlo characterization of a unique nuragic artifact (Sardinia, Italy)

    NASA Astrophysics Data System (ADS)

    Brunetti, Antonio; Depalmas, Anna; di Gennaro, Francesco; Serges, Alessandra; Schiavon, Nicola

    2016-07-01

    The chemical composition of a unique bronze artifact known as the "Cesta" ("Basket") belonging to the ancient Nuragic civilization of the Island of Sardinia, Italy has been analyzed by combining X-ray Fluorescence Spectroscopy (XRF) with Monte Carlo simulations using the XRMC code. The "Cesta" had been discovered probably in the XVIII century with the first graphic representation reported around 1761. In a later draft (dated 1764), the basket has been depicted as being carried upside-down on the shoulder of a large bronze warrior Barthélemy (1761), Pinza (1901), Winckelmann (1776) . The two pictorial representations differed only by the presence of handles in the most recent one. XRF measurements revealed that the handles of the object are composed by brass while the other parts are composed by bronze suggesting the handles as being a later addition to the original object. The artifact is covered at its surface by a fairly thick corrosion patina. In order to determine the bronze bulk composition without the need for removing the outer patina, the artifact has been modeled as a two layer object in Monte Carlo simulations.

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

    NASA Technical Reports Server (NTRS)

    Rolin, T. D.; Leszczuk, Y.

    2008-01-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

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

    PubMed

    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. PMID:25619030

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

    NASA Astrophysics Data System (ADS)

    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.

  19. Rainwater analysis by synchrotron radiation-total reflection X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    López, María L.; Ceppi, Sergio A.; Asar, María L.; Bürgesser, Rodrigo E.; Ávila, Eldo E.

    2015-11-01

    Total reflection X-ray fluorescence analysis excited with synchrotron radiation was used to quantify the elemental concentration of rainwater in Córdoba, Argentina. Standard solutions with gallium as internal standard were prepared for the calibration curves. Rainwater samples of 5 μl were added to an acrylic reflector, allowed to dry, and analyzed for 200 s measuring time. The elemental concentrations of As, Ca, Co, Cr, Cu, Fe, K, Mn, Ni, Pb, S, Sr, V, and Zn were determined. The electrical conductivity, pH, and elemental concentrations were compared to data previously reported for the soluble fraction of rainwater at different sites. A factor analysis was performed in order to determine the sources that contributed to the elemental concentration in rainwater. Anthropogenic sources were identified as traffic pollution, vehicular emissions, and metallurgical factories. The quality of rainwater was analyzed by comparing the concentrations of all the elements in rainwater samples with the WHO guideline values for drinking water. The results show the need to control the atmospheric emissions in order to preserve the quality of rainwater. SR-TXRF analysis of chemical composition of rainwater in Córdoba represents the very first contribution in the region to the knowledge of the concentration of trace metals in the soluble fraction of rainwater. These data are scarce, especially in the Southern Hemisphere.

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

    PubMed

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

    2016-04-01

    Near infrared (NIR) and X-ray fluorescence (XRF) spectroscopy were investigated to predict the concentration of calcium, potassium, iron, magnesium, manganese and zinc in artichoke samples. Sixty artichokes were purchased from different Spanish areas (Benicarló, Valencia and Murcia). NIR and XRF spectra, combined with partial least squares (PLS) data treatment, were used to develop chemometric models for the prediction of mineral concentration. To obtain reference data, samples were mineralised and analysed by inductively coupled plasma optical emission spectrometry (ICP-OES). Coefficients of determination obtained for the regression between predicted values and reference ones for calcium, potassium, magnesium, iron, manganese and zinc were 0.61, 0.79, 0.53, 0.77, 0.54 and 0.60 for NIR and 0.96, 0.93, 0.80, 0.79, 0.76 and 0.90 for XRF, respectively. Both assayed methodologies, offer green alternatives to classical mineral analysis, but XRF provided the best results in order to be used as a quantitative screening method. PMID:26593585

  1. [X-ray fluorescence spectrum studies on bioorganic carbon in cereals and carbon chemical circulation].

    PubMed

    Duan, De-liang; Bian, Fu-yong; Yuan, Bo; Wang, Shu; Ge, Mao-fa; Zhang, Xing-kang; Xu, Si-chuan

    2011-05-01

    The bioorganic carbon contents and chemical element compositions in six kinds of cereals: paddy (rice), wheat (flour), soybean, millet, sorghum and corn were determined by X-ray fluorescence (XRF) spectrum, meanwhile a new method was established to probe their protein contents. In the cereals, the average bioorganic carbon content is about 440%. The highest protein content is 42.74% from soybean, and other protein content is 28.56% in millet, 27.57% in wheat, 24.99% in corn, 22.21% in sorghum, but only 20.31% in rice. Based on our new definition of carbon chemical circulation presented in the current work, the authors have found that in 2009 humankind used bioorganic carbon to discharge CO2 into the earth's atmosphere that accounts for one percent of the total CO2 discharge, and consumed organic carbon to release CO2 into the earth's atmosphere, accounting for 10.73% of the total CO2 discharge. The clear definition of carbon chemical circulation and the discharged CO2 content from the distinct types of carbon compounds would advance the study on carbon chemical circulation and the atmospheric CO2 greenhouse effect. Our work further found that it takes eight years to circulate the total earth's atmospheric CO2. The short period shows the sensitivity for CO2 to keep its dynamical equilibrium in the earth's atmosphere. However, no experimental data has been reported to prove a heavy destructive greenhouse effect of CO2 existing in the earth's atmosphere. PMID:21800615

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

    SciTech Connect

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

    2002-07-29

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

  3. Synchrotron radiation X-ray micro-fluorescence: Protocol to study mesenchymal stem cells.

    PubMed

    Rezende, Karla Mayra; Bönecker, Marcelo; Perez, Carlos Alberto; Mantesso, Andrea

    2016-03-01

    The micro-X-ray fluorescence by synchrotron radiation (μ-XRF) is a method to determine the composition of tissues without destroying the samples. However, this technique has never been used for the analysis of mesenchymal stem cells (MSC). This study compared different protocols for fixing, storing, preserving, and establishing the correct numbers of dental derived MSC submitted to μ-XRF analysis. Stem cells were obtained from human dental tissue. After cell expansion, and MACS isolation, the samples were fixed and the following quantities of cells 1 × 10(4) to 1 × 10(7) were divided in two groups: G1: fixed in 4% paraformaldehyde diluted in phosphate-buffered saline solution, and G2: fixed in 4% paraformaldehyde diluted in MilliQ water. The G1 cells showed precipitation of chemical components from the solution resulting in the formation of salt crystals while G2 cells were clear and almost transparent in the sample holder. With regards to cells concentration, the best results occurred when four droplets of 1 × 10(7) cells were analyzed. This work shows that to identify and study the distribution of trace elements in MSC by μ-XRF, the best protocol is fixation in 4% paraformaldehyde diluted with MilliQ water at 4°C and a concentration of four incremental droplets of 1 × 10(7) cells. PMID:26749077

  4. X-Ray fluorescence measurement of the zinc profile of a single hair

    SciTech Connect

    Toribara, T.Y.; Jackson, D.A.

    1982-04-01

    Many trace elements appear in hair in concentrations related to those in the blood, but the relationship for zinc is complicated by disorders that probably affect its state in the blood. A built-to-order x-ray fluorescence spectrometer was used to measure, nondestructively, the concentrations of 16 elements in a 1-mm interval of a single hair. A scan along a hair strand, together with the known growth rate, enables the zinc concentration in the hair to be correlated with the time the hair was formed. A comparison with the blood concentration at the same time may reveal possible bodily disorders that affect the availability of zinc to incorporation in the hair. The instrument has been carefully calibrated for zinc, and researchers studied the conditions under which there can be losses or gains in the hair after sampling. The sample chamber will accommodate 16 separate holders, and each sample may be automatically measured according to a program pre-selected for it. The average zinc content of hair samples from foreign countries, some ancient specimens, and an interesting profile of a strand from an Iraqi woman are shown.

  5. Evolution of thyroid /sup 127/I stores measured by X-ray fluorescence in subacute thyroiditis

    SciTech Connect

    Fragu, P.; Rougier, P.; Schlumberger, M.; Tubiana, M.

    1982-01-01

    Evaluation of the thyroid iodine content by x-ray fluorescence was performed in 13 patients throughout the course of subacute thyroiditis. In the initial hyperthyroid phase of the disease, the iodine stores of the thyroid were not completely depleted. The iodine content (6.5 +/- 3 mg) was about 2.5 times lower than normal values when thyroiditis had developed in a normal thyroid (10 patients); in 3 patients with goiter; it was elevated (29.6 +/- 6.7 mg) but was still within the normal range of euthyroid goitrous patients. After clinical remission, the iodine content of the gland increased only in two patients (+105% and +43% over the initial value, respectively). For the other patients, the iodine content decreased (from -5% to -100% of the initial value). Restoration of iodine stores occurred subsequently and appeared to be a slow and progressive phenomenon; in six patients the iodine content was still below normal values 12 months after clinical remission (6.6 +/- 1.6 mg). These data suggest that the course of subactue thyroiditis might be longer than would appear from the clinical data, the hormonal assays, or the radioactive thyroid uptake data.

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

    NASA Astrophysics Data System (ADS)

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

    2010-06-01

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

  7. Comparing Compositions of Modern Cast Bronze Sculptures: Optical Emission Spectroscopy Versus x-Ray Fluorescence Spectroscopy

    NASA Astrophysics Data System (ADS)

    Young, M. L.; Dunand, D. C.

    2015-07-01

    Bulk elemental compositions of 74 modern cast bronze sculptures from the collection at the Art Institute of Chicago, the Philadelphia Museum of Art, and the Rodin Museum (Philadelphia, PA) were determined using inductively coupled plasma-optical emission spectroscopy (ICP-OES) and a handheld x-ray fluorescence (XRF) spectrometer. The elemental compositions of the cast sculptures as measured previously by ICP-OES and presently by XRF are compared: A good match is found between the two methods for the base metal (Cu) and the two majority alloying elements (Zn and Sn). For both ICP-OES and XRF data, when the Zn composition is plotted versus the Sn composition, three discernable clusters are found that are related to the artist, foundry, casting date, and casting method; they consist of (A) high-zinc brass, (B) low-zinc, low-tin brass, and (C) low-zinc, tin bronze. Thus, our study confirms that the relatively fast, nondestructive XRF spectrometry can be used effectively over slower and invasive, but more accurate, ICP-OES to help determine a sculpture's artist, foundry, date of creation, date of casting, and casting method.

  8. Quantitative imaging of cell-permeable magnetic resonance contrast agents using x-ray fluorescence.

    PubMed

    Endres, Paul J; Macrenaris, Keith W; Vogt, Stefan; Allen, Matthew J; Meade, Thomas J

    2006-01-01

    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-dimethylamino)stilbene. 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 10(3) better than (153)Gd gamma counting, without altering the agent by organic fluorophore conjugation. The transduction efficiency of the intracellular agents was evaluated by T(1) analysis and inductively coupled plasma mass spectrometry to determine the efficacy of each chelate-transporter combination. PMID:17150161

  9. Using synchrotron X-ray fluorescence microprobes in the study of metal homeostasis in plants

    PubMed Central

    Punshon, Tracy; Guerinot, Mary Lou; Lanzirotti, Antonio

    2009-01-01

    Background and Aims This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis. PMID:19182222

  10. Micro energy-dispersive x-ray fluorescence spectrometry study of dentin coating with nanobiomaterials

    NASA Astrophysics Data System (ADS)

    Soares, Luís. Eduardo Silva; Nahorny, Sídnei; Marciano, Fernanda Roberta; Zanin, Hudson; Lobo, Anderson de Oliveira

    2015-06-01

    New biomaterials such as multi-walled carbon nanotubes oxide/graphene oxide (MWCNTO/GO), nanohydroxyapatite (nHAp) and combination of them together or not to acidulated phosphate fluoride gel (F) have been tested as protective coating before root dentin erosion. Fourteen bovine teeth were cleaned, polished, divided into two parts (n=28) and assigned to seven groups: (Control) - without previous surface treatment; F treatment; nHAp; MWCNTO/GO; F+nHAp; F+MWCNTO/GO and F+MWCNTO/GO/nHAp composites. Each sample had two sites of pre-treatments: acid etched area and an area without treatment. After the biomaterials application, the samples were submitted to six cycles (demineralization: orange juice, 10 min; remineralization: artificial saliva, 1 h). Micro energy-dispersive X-ray fluorescence spectrometry (μ-EDXRF) mapping area analyses were performed after erosive cycling on both sites (n=84). μ-EDXRF mappings showed that artificial saliva and MWCNTO/GO/nHAp/F composite treatments produced lower dentin demineralization than in the other groups. Exposed dentin tubules allowed better interaction of nanobiomaterials than in smear layer covered dentin. Association of fluoride with other biomaterials had a positive influence on acid etched dentin. MWCNTO/GO/nHAp/F composite treatment resulted in levels of demineralization similar to the control group.

  11. Using Synchrotron X-ray Fluorescence Microprobes in the Study of Metal Homeostasis in Plants

    SciTech Connect

    Punshon, T.; Guerinot, M; Lanzirotti, A

    2009-01-01

    Background and Aims: This Botanical Briefing reviews the application of synchrotron X-ray fluorescence (SXRF) microprobes to the plant sciences; how the technique has expanded our knowledge of metal(loid) homeostasis, and how it can be used in the future. Scope: The use of SXRF microspectroscopy and microtomography in research on metal homeostasis in plants is reviewed. The potential use of SXRF as part of the ionomics toolbox, where it is able to provide fundamental information on the way that plants control metal homeostasis, is recommended. Conclusions: SXRF is one of the few techniques capable of providing spatially resolved in-vivo metal abundance data on a sub-micrometre scale, without the need for chemical fixation, coating, drying or even sectioning of samples. This gives researchers the ability to uncover mechanisms of plant metal homeostasis that can potentially be obscured by the artefacts of sample preparation. Further, new generation synchrotrons with smaller beam sizes and more sensitive detection systems will allow for the imaging of metal distribution within single living plant cells. Even greater advances in our understanding of metal homeostasis in plants can be gained by overcoming some of the practical boundaries that exist in the use of SXRF analysis.

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  13. Composite silica coated gold nanosphere and quantum dots nanoparticles for X-ray CT and fluorescence bimodal imaging.

    PubMed

    Song, Ji-Tao; Yang, Xiao-Quan; Zhang, Xiao-Shuai; Yan, Dong-Mei; Yao, Ming-Hao; Qin, Meng-Yao; Zhao, Yuan-Di

    2015-07-01

    In this study, silica coated Au nanospheres (Au@SiO2) were prepared by a reverse microemulsion method; subsequently, a layer of fluorescent quantum dots (QDs) were adsorbed onto it and then it was coated with silica again. After modifying with PVP, the composite silica coated gold nanosphere and quantum dots nanoparticle (Au@SiO2-QDs/SiO2-PVP) was obtained. This composite structure contained Au and QDs, and it could be used for contrast-enhanced X-ray CT imaging and fluorescence imaging. Characterization showed that the composite nanoparticle had good dispersity, a high fluorescence intensity and a good effect of X-ray absorption, and it was suitable for using as a bimodal imaging probe. PMID:26008798

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

    NASA Astrophysics Data System (ADS)

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

    2007-10-01

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

  15. Speciation and localization of Zn in the hyperaccumulator Sedum alfredii by extended X-ray absorption fine structure and micro-X-ray fluorescence.

    PubMed

    Lu, Lingli; Liao, Xingcheng; Labavitch, John; Yang, Xiaoe; Nelson, Erik; Du, Yonghua; Brown, Patrick H; Tian, Shengke

    2014-11-01

    Differences in metal homeostasis among related plant species can give important information of metal hyperaccumulation mechanisms. Speciation and distribution of Zn were investigated in a hyperaccumulating population of Sedum alfredii by using extended X-ray absorption fine structure and micro-synchrotron X-ray fluorescence (μ-XRF), respectively. The hyperaccumulator uses complexation with oxygen donor ligands for Zn storage in leaves and stems, and variations in the Zn speciation was noted in different tissues. The dominant chemical form of Zn in leaves was most probably a complex with malate, the most prevalent organic acid in S. alfredii leaves. In stems, Zn was mainly associated with malate and cell walls, while Zn-citrate and Zn-cell wall complexes dominated in the roots. Two-dimensional μ-XRF images revealed age-dependent differences in Zn localization in S. alfredii stems and leaves. In old leaves of S. alfredii, Zn was high in the midrib, margin regions and the petiole, whereas distribution of Zn was essentially uniform in young leaves. Zinc was preferentially sequestered by cells near vascular bundles in young stems, but was highly localized to vascular bundles and the outer cortex layer of old stems. The results suggest that tissue- and age-dependent variations of Zn speciation and distribution occurred in the hyperaccumulator S. alfredii, with most of the Zn complexed with malate in the leaves, but a shift to cell wall- and citric acid-Zn complexes during transportation and storage in stems and roots. This implies that biotransformation in Zn complexation occurred during transportation and storage processes in the plants of S. alfredii. PMID:25306525

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

    NASA Astrophysics Data System (ADS)

    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 ( P<0.001) and 0.87( P<0.03) times 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

  17. X-ray fluorescence spectrometry using Synchrotron Radiation with applications in unmanned aircraft environmental sensing

    NASA Astrophysics Data System (ADS)

    Barberie, Sean Richard Gopal

    In this thesis I present an analytical optimization of the Synchrotron Radiation X-Ray Fluorescence (SR-XRF) technique for applications in unmanned aircraft aerosol studies. In environmental and atmospheric science, there is a pressing need for aerosol measurements at various altitudes in the atmosphere and spanning large regions. This need is currently either ignored, or met to a limited degree by studies that employ manned aircraft. There is, however, a great deal of opportunity to improve and expand on these studies using the emerging technology of unmanned aircraft systems. A newly developed aerosol sampler makes this opportunity a near-reality by its ability to collect aerosol samples in-situ from unmanned aircraft platforms. The challenge lies in analyzing these samples for elemental composition. In airborne aerosol studies, the ability to resolve where a sample was collected both spatially and temporally is limited by the sensitivity of the analysis technique. In aircraft-based aerosol collection, the length of the aerosol sample spot corresponds to distance. Thus the spatial resolution of an airborne study is limited by the amount of mass that must be collected for analysis. The SR-XRF optimizations outlined in this thesis decrease the amount of sample mass required for detectable elemental concentrations, allowing aerosol samples to be analyzed in smaller areas corresponding to smaller time steps. Since, in a flight path, time steps are directly correlated with distance, analysis of smaller time steps results in the ability to measure aerosols at higher spatial resolution. Four SR-XRF analysis configurations were experimentally tested: monochromatic beam, white beam, filtered white beam, and filtered white beam-filtered detector to determine which configuration gave the highest elemental sensitivity and selectivity. Of these tested methods, the straight polychromatic white beam configuration resulted in the best sensitivity for elements across a large

  18. TU-F-18A-05: An X-Ray Fluorescence Technique for Energy Calibration of Photon-Counting Detectors

    SciTech Connect

    Ding, H; Cho, H; Molloi, S; Barber, W; Iwanczyk, J

    2014-06-15

    Purpose: To investigate the feasibility of energy response calibration of a Si strip photon-counting detector by using the x-ray fluorescence technique. Methods: X-ray fluorescence was generated by using a pencil beam from a tungsten anode x-ray tube with 2 mm Al filtration. Spectra were acquired at 90° from the primary beam direction with an energy-resolved photon-counting detector based on Si strips. The distances from the source to target and the target to detector were approximately 19 and 11 cm, respectively. Four different materials, containing Ag, I, Ba, and Gd, were placed in small plastic aliquots with a diameter of approximately 0.7 cm for x-ray fluorescence measurements. Linear regression analysis was performed to derive the gain and offset values for the correlation between the measured fluorescence peak center and the known energies for materials. The energy resolution was derived from the full width at half maximum (FWHM) of the fluorescence peaks. In addition, the angular dependence of the recorded fluorescence spectra was studied at 30°, 60°, and 120°. Results: Strong fluorescence signals of all four target materials were recorded with the investigated geometry for the Si strip detector. The recorded pulse height was calibrated with respect to photon energy and the gain and offset values were calculated to be 7.0 mV/keV and −69.3 mV, respectively. Negligible variation in energy calibration was observed among the four energy thresholds. The variation among different pixels was estimated to be approximately 1 keV. The energy resolution of the detector was estimated to be 7.9% within the investigated energy range. Conclusion: The performance of a spectral imaging system using energy-resolved photon-counting detectors is very dependent on the energy calibration of the detector. The proposed x-ray fluorescence technique provides an accurate and efficient way to calibrate the energy response of a photon-counting detector.

  19. The Application of Synchrotron X-ray Fluorescence to Dendroanalysis: Nickel in Salix nigra L.

    NASA Astrophysics Data System (ADS)

    Punshon, T.; Bertsch, P. M.; Lanzirotti, A.; McLeod, K. W.; Burger, J.

    2003-12-01

    Synchotron X-ray Fluorescence microanalysis (SXRF) has been applied to annual rings of willows (Salix nigra L.) collected from an eroding former radiological settling basin and the impacted depositional area downstream. In 1984 the enclosing spillway of Steed Pond breached, and a pulse of U and Ni contaminated sediments moved downstream, accumulating in Lower Tims Branch (LTB), continuing during storm events. The aim of the study was to correlate fluctuations in contaminant concentrations within annual rings of impacted trees with the contaminant history, specifically the major contaminant pulse of 1984. Trees were sampled at Steed Pond, LTB and an uncontaminated reference site. Their rings were measured, aged and sectioned for SXRF analysis. Analysis took several forms: one-dimensional line scans (from pith to cambium) to show fluctuations in metal concentration over the lifetime of the tree; two-dimensional elemental maps to show metal distribution between and within annual rings, and three-dimension fluorescence tomography, to show the structure and composition of regions of interest. Trees from LTB clearly showed a marked increase in Ni concentration within the annual ring formed in 1984, and a series of peaks in subsequent years. Notably, lesser contaminants Cu, Zn and Cr showed an identical pattern. U was not present. Compositional mapping showed Ni associated with annual rings, with a clear demarcation between rings. Closer examination revealed smaller areas (10 to 20 microns in diameter) containing approximately 1000 ppm Ni. These discrete areas were exclusively Ni containing features, and were examined further with three-dimensional fluorescence tomography, showing that the Ni features occurred inside the lumen of vessel elements. We concluded that the Ni signature in annual rings of willows from LTB correlated with known contaminant pulses. Further, the technique quantitatively distinguished between trees growing on the radiological settling pond (having

  20. Forensic analysis of laser printed ink by X-ray fluorescence and laser-excited plume fluorescence.

    PubMed

    Chu, Po-Chun; Cai, Bruno Yue; Tsoi, Yeuk Ki; Yuen, Ronald; Leung, Kelvin S Y; Cheung, Nai-Ho

    2013-05-01

    We demonstrated a minimally destructive two-tier approach for multielement forensic analysis of laser-printed ink. The printed document was first screened using a portable-X-ray fluorescence (XRF) probe. If the results were not conclusive, a laser microprobe was then deployed. The laser probe was based on a two-pulse scheme: the first laser pulse ablated a thin layer of the printed ink; the second laser pulse at 193 nm induced multianalytes in the desorbed ink to fluoresce. We analyzed four brands of black toners. The toners were printed on paper in the form of patches or letters or overprinted on another ink. The XRF probe could sort the four brands if the printed letters were larger than font 20. It could not tell the printing sequence in the case of overprints. The laser probe was more discriminatory; it could sort the toner brands and reveal the overprint sequence regardless of font size while the sampled area was not visibly different from neighboring areas even under the microscope. In terms of general analytical performance, the laser probe featured tens of micrometer lateral resolution and tens to hundreds of nm depth resolution and atto-mole mass detection limits. It could handle samples of arbitrary size and shape and was air compatible, and no sample pretreatment was necessary. It will prove useful whenever high-resolution and high sensitivity 3D elemental mapping is required. PMID:23570307

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

    NASA Astrophysics Data System (ADS)

    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

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

    PubMed

    Twining, Benjamin S; Baines, Stephen B; Fisher, Nicholas S; Maser, Jörg; Vogt, Stefan; Jacobsen, Chris; Tovar-Sanchez, Antonio; Sañudo-Wilhelmy, Sergio A

    2003-08-01

    The study of trace metal cycling by aquatic protists is limited by current analytical techniques. Standard "bulk" element analysis techniques that rely on physical separations to concentrate cells for analysis cannot separate cells from co-occurring detrital material or other cells of differing taxonomy or trophic function. Here we demonstrate the ability of a synchrotron-based X-ray fluorescence (SXRF) microprobe to quantify the elements Si, Mn, Fe, Ni, and Zn in individual aquatic protist cells. This technique distinguishes between different types of cells in an assemblage and between cells and other particulate matter. Under typical operating conditions, the minimum detection limits are 7.0 x 10(-16) mol microm(-2) for Si and between 5.0 x 10(-20) and 3.9 x 10(-19) mol microm(-2) for Mn, Fe, Ni, and Zn; this sensitivity is sufficient to detect these elements in cells from even the most pristine waters as demonstrated in phytoplankton cells collected from remote areas of the Southern Ocean. Replicate analyses of single cells produced variations of <5% for Si, Mn, Fe, and Zn and <10% for Ni. Comparative analyses of cultured phytoplankton cells generally show no significant differences in cellular metal concentrations measured with SXRF and standard bulk techniques (spectrophotometry and graphite furnace atomic absorption spectrometry). SXRF also produces two-dimensional maps of element distributions in cells, thereby providing information not available with other analytical approaches. This technique enables the accurate and precise measurement of trace metals in individual aquatic protists collected from natural environments. PMID:14572047

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

    NASA Astrophysics Data System (ADS)

    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.

  4. X-ray fluorescence analysis of rare earth elements in rocks using low dilution glass beads.

    PubMed

    Nakayama, Kenichi; Nakamura, Toshihiro

    2005-07-01

    Major and trace elements (Na, Mg, Al, Si, P, K, Ca, Ti, Mn, Fe, Rb, Sr, Y, Zr, La, Ce, Pr, Nd, Sm, Gd, Dy, Th and U) in igneous rocks were assayed with fused lithium borate glass beads using X-ray fluorescence spectrometry. Low dilution glass beads, which had a 1:1 sample-to-flux ratio, were prepared for determination of rare earth elements. Complete vitrification of 1:1 mixture required heating twice at 1200 degrees C with agitation. Extra pure reagents containing determinants were used for calibrating standards instead of the rock standard. The calibration curves of the 23 elements showed good linearity. Furthermore, the lower limits of detection corresponding to three times the standard deviation for blank measurements were 26 mass ppm for Na2O, 6.7 for MgO, 4.5 for Al2O3, 4.5 for SiO2, 18 for P2O5, 1.1 for K2O, 4.0 for CaO, 3.9 for TiO2, 1.6 for MnO, 0.8 for Fe2O3, 0.5 for Rb, 0.2 for Sr, 0.4 for Y, 0.5 for Zr, 3.3 for La, 6.5 for Ce, 2.7 for Pr, 2.1 for Nd, 1.7 for Sm, 0.7 for Gd, 2.7 for Dy, 0.5 for Th, and 0.6 for U. Using the present method, we determined the contents of these 23 elements in four rhyolitic and granitic rocks from Japan. PMID:16038502

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

    SciTech Connect

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

    2003-01-01

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

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

    PubMed Central

    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

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

    PubMed

    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. PMID:26536141

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

    SciTech Connect

    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}.

  9. Rare earth element concentrations in geological and synthetic samples using synchrotron X-ray fluorescence analysis

    USGS Publications Warehouse

    Chen, J.R.; Chao, E.C.T.; Back, J.M.; Minkin, J.A.; Rivers, M.L.; Sutton, S.R.; Cygan, G.L.; Grossman, J.N.; Reed, M.J.

    1993-01-01

    The concentrations of rare earth elements (REEs) in specific mineral grains from the Bayan Obo ore deposit and synthetic high-silica glass samples have been measured by synchrotron X-ray fluorescence (SXRF) analysis using excitation of the REE K lines between 33 and 63 keV. Because SXRF, a nondestructive analytical technique, has much lower minimum detection limits (MDLs) for REEs, it is an important device that extends the in situ analytical capability of electron probe microanalysis (EPMA). The distribution of trace amounts of REEs in common rock-forming minerals, as well as in REE minerals and minerals having minor quantities of REEs, can be analyzed with SXRF. Synchrotron radiation from a bending magnet and a wiggler source at the National Synchrotron Light Source, Brookhaven National Laboratory, was used to excite the REEs. MDLs of 6 ppm (La) to 26 ppm (Lu) for 3600 s in 60-??m-thick standard samples were obtained with a 25-??m diameter wiggler beam. The MDLs for the light REEs were a factor of 10-20 lower than the MDLs obtained with a bending magnet beam. The SXRF REE concentrations in mineral grains greater than 25 ??m compared favorably with measurements using EPMA. Because EPMA offered REE MDLs as low as several hundred ppm, the comparison was limited to the abundant light REEs (La, Ce, Pr, Nd). For trace values of medium and heavy REEs, the SXRF concentrations were in good agreement with measurements using instrumental neutron activation analysis (INAA), a bulk analysis technique. ?? 1993.

  10. Trace element abundances in single presolar silicon carbide grains by synchrotron X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Kashiv, Yoav

    2004-12-01

    Synchrotron x-ray fluorescence (SXRF) was applied to the study of presolar grains for the first time in this study. 41 single SiC grains of the KJF size fraction (mass-weighted median size of 1.86 μm) from the Murchison (CM2) Meteorite were analyzed. The absolute abundances of the following elements were determined (not every element in every grain): S, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Sr, Y, Zr, Nb, Mo, Ru, Os, Ir and Pt (underlined elements were detected here for the first time in single grains). There is good agreement between the heavier trace element abundances in the grains and s-process nucleosynthesis calculations. It suggests that smaller 13C pocket sizes are needed in the parent stars, a free parameter in the stellar models, than is deduced from isotopic analyses of s-, and s-mainly, elements, such as Zr and Mo. In addition, the data confirms the radiogenic nature of the Nb in the grains, due to the in situ decay of 93Zr (t 1/2 = 1.5 × 106 year). The data suggest that the trace elements condensed into the host SiC grains by a combination of condensation in solid solution and incorporation of subgrains. It seems that many of the trace elements reside mainly in subgrains of two solid solution: (1)a TiC based solid solution, and (2)a Mo-Ru carbide based solid solution. The presence of subgrains of an Fe-Ni alloy solid solution is suggested as well. Subgrains of all 3 solid solutions were observed previously in presolar graphite grains.* *This dissertation is a compound document (contains both a paper copy and a CD as part of the dissertation). The CD requires the following system requirements: Adobe Acrobat.

  11. X-ray Fluorescence Imaging of the Hippocampal Formation After Manganese Exposure†

    PubMed Central

    Robison, Gregory; Zakharova, Taisiya; Fu, Sherleen; Jiang, Wendy; Fulper, Rachael; Barrea, Raul; Zheng, Wei; Pushkar, Yulia

    2013-01-01

    Manganese (Mn) intoxication results in neurological conditions similar, but not identical, to idiopathic Parkinson’s disease. While the mechanism(s) by which Mn exposure leads to neurotoxic effects remains unclear, studies by magnetic resonance imaging demonstrate a high Mn accumulation in the hippocampal formation (HPCf) of the brain. Metal quantification using this method is not possible. Using x-ray fluorescence imaging, we measured the distribution of Mn in the HPCf for a rodent model of chronic Mn exposure and quantitatively compared it with distributions of other biologically relevant metals. We found considerable increases in average Mn concentrations in all analyzed areas and we identified the dentate gyrus (DG) and the cornus ammonis 3 (CA3) layer as areas accumulating the highest Mn content (~1.2 µg Mn/g tissue). The DG is significantly enriched with iron (Fe), while the CA3 layer has high zinc (Zn) content. Additionally, significant spatial correlations were found for Mn/Zn concentrations across the identified substructures of the HPCf and for Mn/Fe concentrations in the DG. Combined results support that at least two mechanisms may be responsible for Mn transport and/or storage in the brain, associated with either Fe or Zn. Subcellular resolution images of metal distribution in cells of the CA3 show diffuse Mn distributions consistent with Mn localization in both the cytoplasm and nucleus. Mn was not increased in localized intracellular Fe or copper accumulations. A consistent Mn/Zn correlation both at the tissue (40 µm × 40 µm) and cellular (0.3 µm × 0.3 µm) levels suggests that a Zn transport/storage mechanism in the HPCf is likely associated with Mn accumulation. PMID:23999853

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

    SciTech Connect

    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.

  13. X-Ray Fluorescence Imaging: A New Tool for Studying Manganese Neurotoxicity

    PubMed Central

    Robison, Gregory; Zakharova, Taisiya; Fu, Sherleen; Jiang, Wendy; Fulper, Rachael; Barrea, Raul; Marcus, Matthew A.; Zheng, Wei; Pushkar, Yulia

    2012-01-01

    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. PMID:23185282

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

    PubMed

    Colvin, Robert A; Jin, Qiaoling; Lai, Barry; Kiedrowski, Lech

    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

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

    PubMed

    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

  16. Transmission-corrected x-ray fluorescence analysis of uranium and plutonium solutions using a dual transmission source

    SciTech Connect

    Ruhter, W.D.; Camp, D.C.

    1987-11-24

    The energy-dispersive x-ray fluorescence analysis (XRFA) technique has been implemented at several spent nuclear fuel reprocessing facilities for nondestructive measurements of uranium and/or plutonium concentrations in process streams and product storage tanks. An important factor in these quantitative measurements is the absorption of the fluoresced x-rays by the solution matrix, which must be taken into account to accurately quantify the U or Pu concentrations. We describe a new, accurate method using a dual transmission source of Gd-153 and Co-57 to correct for matrix effects. Results of measurements on uranium and plutonium solution standards show the methodology to be better than 0.5%, which includes statistical precision, over the concentration range from 1 to 250 g/l. 5 refs., 4 figs., 3 tabs.

  17. Asymmetric Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

    SciTech Connect

    Popescu, B.F.Gh.; Belak, Z.R.; Ignatyev, K.; Ovsenek, N.; Nichol, H.

    2009-06-04

    The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was also concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.

  18. Asymmetri Distribution of Metals in the Xenopus Laevis Oocyte: a Synchrotron X-Ray Fluorescence Microprobe Study

    SciTech Connect

    Popescu, B.F.G.; Belak, Z.R.; Ignatyev, K.; Ovsenek, N.; Nichol, H.; /Saskatchewan U. /SLAC, SSRL

    2009-04-29

    The asymmetric distribution of many components of the Xenopus oocyte, including RNA, proteins, and pigment, provides a framework for cellular specialization during development. During maturation, Xenopus oocytes also acquire metals needed for development, but apart from zinc, little is known about their distribution. Synchrotron X-ray fluorescence microprobe was used to map iron, copper, and zinc and the metalloid selenium in a whole oocyte. Iron, zinc, and copper were asymmetrically distributed in the cytoplasm, while selenium and copper were more abundant in the nucleus. A zone of high copper and zinc was seen in the animal pole cytoplasm. Iron was also concentrated in the animal pole but did not colocalize with zinc, copper, or pigment accumulations. This asymmetry of metal deposition may be important for normal development. Synchrotron X-ray fluorescence microprobe will be a useful tool to examine how metals accumulate and redistribute during fertilization and embryonic development.

  19. Special tablets containing cellulose binder and Sr internal standard for simplifying X-ray fluorescence analysis of powder samples

    NASA Astrophysics Data System (ADS)

    Mzyk, Zofia; Anyszkiewicz, Jacek; Gorewoda, Tadeusz

    2015-12-01

    The addition of a constant amount of SrCO3 was observed to be the proper internal standard for analysis by wavelength-dispersive X-ray fluorescence spectrometry to correct the matrix and grain size effects of many constituents. The weighing of constant amounts of SrCO3, binder and sample allowed for the preparation time for analysis to be extended, and special tablets containing binder and SrCO3 were developed. Several substances were tested as binders, among which microcrystalline cellulose was chosen for further study. The prepared tablets were checked for their weight stability and the repeatability of SrCO3 addition. The tablets were then used to prepare pellets from geological samples for X-ray fluorescence analysis. The exemplary application and calibration curves for several analytes confirmed that the prepared tablets could be useful for the pelletizing of such materials to compensate for matrix effects.

  20. Elemental analysis with a full-field X-ray fluorescence microscope and a CCD photon-counting system.

    PubMed

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

    2002-05-01

    The first result is presented of an X-ray fluorescence microscope with a Wolter mirror in combination with a CCD camera used as an energy-resolved two-dimensional detector in photon-counting mode. Two-dimensional elemental maps of metallic wires, such as Fe, Co, Ni and Cu, and inclusions of a synthesized diamond could be obtained with an energy resolution of 350 eV. PMID:11972365

  1. Magnetic circular dichroism in the X-ray fluorescence spectra of iron and a glassy-metal iron alloy

    NASA Astrophysics Data System (ADS)

    Hague, C. F.; Mariot, J.-M.

    1995-05-01

    Magnetic circular dichroism (MCD) in the X-ray fluorescence of iron has been examined using white bending magnet radiation at Super-ACO. A new spectrometer fitted with a position sensitive detector provided data with improved statistics compared to earlier results. The origin of a dip observed in the Lα dichroic signal but not in the Lβ dichroic signal is reinterpreted. As a guide to interpretation we have also measured the MCD of glassy FeNiBMo.

  2. An analysis of lead, bromine, zinc and sulphur in airborne participate matter by x-ray fluorescence spectroscopy

    SciTech Connect

    McKee, J.S.C.; Lapointe, C.; Wise, M.L.H.

    1980-01-01

    Research report: Atmospheric concentrations of lead, bromine, zinc, and sulfur were measured daily for 7 mo at two sites in Birmingham, England. Samples collected at a highway location and at an inland site were analyzed by X-ray fluorescence spectroscopy. Atmospheric levels of the pollutants are higher at the highway site than at the inland site, demonstrating the polluting effects of vehicular traffic. Particulate sizes were also determined. (1 map, 4 photos, 19 references, 1 table)

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

    ERIC Educational Resources Information Center

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

    2011-01-01

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

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

    SciTech Connect

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

    2015-03-15

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

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

    PubMed

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

    2015-03-01

    X-ray absorption fine structure (XAFS) measurements are widely used for the analysis of electronic structure. Generally, XAFS in the soft X-ray region is measured under vacuum, but chemical structures under vacuum are typically different from those under operando conditions, where chemical species exhibit their function. Here, we developed an XAFS measurement instrument, as a step toward operando fluorescent, which yields XAFS measurement using synchrotron radiation in the soft X-ray region. We applied this method to analyze the local electronic structure of the sulfur atoms in L-cysteine in different pH solutions. In water at pH 7, the hydrogen atom does not dissociate from the thiol (-SH) group in L-cysteine, which forms a structure surrounded by and interacting with water molecules. The XAFS spectrum of L-cysteine in solution was altered by changing the pH. At pH 9, the hydrogen atom dissociated and a thiolate anion was formed. Although the -SH group was oxidized to SO4 (2-) when L-cysteine was adsorbed on a metal surface and dried, no oxidation was observed in solution. This may be because the water molecules were densely packed and protected the -SH group from oxidation. Our results show that this instrument aimed toward operando fluorescence XAFS measurements in the soft X-ray region is useful for structural analysis of sulfur atoms in organic molecules in air and in solution. The instrument will be applied to the structural analysis of materials containing elements that have absorption edges in soft X-ray region, such as phosphorus and alkali metals (potassium and cesium). It will be also particularly useful for the analysis of samples that are difficult to handle under vacuum and materials that have specific functions in solution. PMID:25832271

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

    NASA Astrophysics Data System (ADS)

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

    2015-03-01

    X-ray absorption fine structure (XAFS) measurements are widely used for the analysis of electronic structure. Generally, XAFS in the soft X-ray region is measured under vacuum, but chemical structures under vacuum are typically different from those under operando conditions, where chemical species exhibit their function. Here, we developed an XAFS measurement instrument, as a step toward operando fluorescent, which yields XAFS measurement using synchrotron radiation in the soft X-ray region. We applied this method to analyze the local electronic structure of the sulfur atoms in L-cysteine in different pH solutions. In water at pH 7, the hydrogen atom does not dissociate from the thiol (-SH) group in L-cysteine, which forms a structure surrounded by and interacting with water molecules. The XAFS spectrum of L-cysteine in solution was altered by changing the pH. At pH 9, the hydrogen atom dissociated and a thiolate anion was formed. Although the -SH group was oxidized to SO42- when L-cysteine was adsorbed on a metal surface and dried, no oxidation was observed in solution. This may be because the water molecules were densely packed and protected the -SH group from oxidation. Our results show that this instrument aimed toward operando fluorescence XAFS measurements in the soft X-ray region is useful for structural analysis of sulfur atoms in organic molecules in air and in solution. The instrument will be applied to the structural analysis of materials containing elements that have absorption edges in soft X-ray region, such as phosphorus and alkali metals (potassium and cesium). It will be also particularly useful for the analysis of samples that are difficult to handle under vacuum and materials that have specific functions in solution.

  7. Improved signal-to-noise ratio for non-perpendicular detection angles in x-ray fluorescence computed tomography (XFCT).

    PubMed

    Sjölin, Martin; Danielsson, Mats

    2014-11-01

    The standard imaging setup in x-ray fluorescence computed tomography detects the fluorescence emission at a right angle with respect to the axis of the excitation beam. In this paper we have studied how the detection angle affects the signal-to-noise ratio (S/N), which is a major factor influencing the low-contrast sensitivity of the imaging system. This is done for an imaging setup using a collimated detector and a pencil beam of excitation x-rays. An ideal detection process is simulated for a generalized imaging case with gold/platinum tracers and experimental measurements are performed using a diagnostic x-ray tube. For monochromatic excitation, the results indicate that order-of-magnitude improvements of the S/N can be achieved by optimizing the detection angle. The maximal S/N, when exciting with an energy just above the K-edge, is achieved for large detection angles, i.e. with the detector close to the source. The improvements also transfer to polychromatic excitation sources and the experimental results show up to four-fold improvements of the S/N when changing the detection angle from 90° to 150°. Also, the changes of the S/N behavior when switching the fluorescent tracer is briefly demonstrated. These results suggest that the choice of detection angle should be taken seriously in the design of future XFCT imaging systems. PMID:25310695

  8. Improved signal-to-noise ratio for non-perpendicular detection angles in x-ray fluorescence computed tomography (XFCT)

    NASA Astrophysics Data System (ADS)

    Sjölin, Martin; Danielsson, Mats

    2014-11-01

    The standard imaging setup in x-ray fluorescence computed tomography detects the fluorescence emission at a right angle with respect to the axis of the excitation beam. In this paper we have studied how the detection angle affects the signal-to-noise ratio (S/N), which is a major factor influencing the low-contrast sensitivity of the imaging system. This is done for an imaging setup using a collimated detector and a pencil beam of excitation x-rays. An ideal detection process is simulated for a generalized imaging case with gold/platinum tracers and experimental measurements are performed using a diagnostic x-ray tube. For monochromatic excitation, the results indicate that order-of-magnitude improvements of the S/N can be achieved by optimizing the detection angle. The maximal S/N, when exciting with an energy just above the K-edge, is achieved for large detection angles, i.e. with the detector close to the source. The improvements also transfer to polychromatic excitation sources and the experimental results show up to four-fold improvements of the S/N when changing the detection angle from 90° to 150°. Also, the changes of the S/N behavior when switching the fluorescent tracer is briefly demonstrated. These results suggest that the choice of detection angle should be taken seriously in the design of future XFCT imaging systems.

  9. Development of a new Planetary SCD-based X-Ray Fluorescence Spectrometer Package for in-situ Analysis

    NASA Astrophysics Data System (ADS)

    Fabel, Oliver; Köhler, Eberhard; Dreißigacker, Anne; Meyer, Matthias; van Gasselt, Stephan

    2014-05-01

    We propose an X-Ray Fluorescence Instrument Package (XRF-X and XRF-ISM) in order to measure the composition of rock-surface materials from orbiter, lander, and rover-based systems directly and quantitatively. It is suited for all future missions to the Moon, but also to the Galilean Satellites or any other solid-surface solar system body without an atmosphere. Collected data will be used for constructing detailed geochemical maps of the target body's surface composition. The typical spectral range is 1 - 10 keV (1.2 - 0.12 nm) with no sharp limits, achieving a spectral resolution of 160 eV at 6 keV. At these conditions, elemental abundances of lighter elements (atomic no. 11-32, K-Lines) and heavier elements (atomic no. 33-80, L-lines) will be observable. This will allow for mapping concentrations of the main mineral- (and therefore rock-) forming elements of surface materials, in particular Na, Mg, Al, Si, K, Ca, Ti, Mn, and Fe. The spatial resolution (GSD) is 10 km/px at an orbit altitude of 50 km. The package consists of two subsystems: (1) the main instrument targeting at a body's surface (XRF-X), and (2) a zenith-pointing solar monitor which incorporates calibration targets for taking account of solar X-Rays and particles (XRF-ISM). Both instruments make use of Energy-Dispersive X-Ray Fluorescence (EDX) with solar X-Ray excitation to probe materials over arbitrary distances. By monitoring incident Solar X-Ray and potential particle flux through synchronous measurement of a calibration target, XRF-X measurements can be obtained even over long distances, e.g. from a lunar orbiter. A scalable and modular design allows for instrument adaptions to desired resolution, to weight and power-consumption constraints and to expected sun emission intensities. The design will also allow adaption for employment on different observation platforms. In the current laboratory setup, both experiments are developed using large-area swept charge devices (SCD) to allow for high X-Ray

  10. 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.

    PubMed

    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

  11. Simultaneous determination of thorium, niobium, lead, and zinc by photon-induced x-ray fluorescence of lateritic material

    SciTech Connect

    LaBrecque, J.J.; Adames, D.; Parker, W.C.

    1981-01-01

    A rapid method is presented for the simultaneous determinations of thorium, niobium, lead, and zinc in lateritic material from Cerro Impacto, Estado Bolivar, Venezuela. This technique uses a PDP - 11/05 processor - based photon induced x-ray fluorescence system. The total variations of approximately 5% for concentrations of approximately 1 and 10% for concentrations of approximately 0.1% were obtained with only 500 s of fluorescent time. The values obtained by this method were in agreement with values measured by conventional flame atomic absorption spectroscopy for lead and zinc. The values for thorium measured were in agreement with the reported values for the reference materials supplied by NBL.

  12. Identifying Objects via Encased X-Ray-Fluorescent Materials - the Bar Code Inside

    NASA Technical Reports Server (NTRS)

    Schramm, Harry F.; Kaiser, Bruce

    2005-01-01

    Systems for identifying objects by means of x-ray fluorescence (XRF) of encased labeling elements have been developed. The XRF spectra of objects so labeled would be analogous to the external bar code labels now used to track objects in everyday commerce. In conjunction with computer-based tracking systems, databases, and labeling conventions, the XRF labels could be used in essentially the same manner as that of bar codes to track inventories and to record and process commercial transactions. In addition, as summarized briefly below, embedded XRF labels could be used to verify the authenticity of products, thereby helping to deter counterfeiting and fraud. A system, as described above, is called an encased core product identification and authentication system (ECPIAS). The ECPIAS concept is a modified version of that of a related recently initiated commercial development of handheld XRF spectral scanners that would identify alloys or detect labeling elements deposited on the surfaces of objects. In contrast, an ECPIAS would utilize labeling elements encased within the objects of interest. The basic ECPIAS concept is best illustrated by means of an example of one of several potential applications: labeling of cultured pearls by labeling the seed particles implanted in oysters to grow the pearls. Each pearl farmer would be assigned a unique mixture of labeling elements that could be distinguished from the corresponding mixtures of other farmers. The mixture would be either incorporated into or applied to the surfaces of the seed prior to implantation in the oyster. If necessary, the labeled seed would be further coated to make it nontoxic to the oyster. After implantation, the growth of layers of mother of pearl on the seed would encase the XRF labels, making these labels integral, permanent parts of the pearls that could not be removed without destroying the pearls themselves. The XRF labels would be read by use of XRF scanners, the spectral data outputs of which

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

    SciTech Connect

    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 to

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

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

    PubMed

    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. Results with a >30% error were found in samples which contained very low or very

  16. Evaluation of the uncertainties associated with in vivo X-ray fluorescence bone lead calibrations

    NASA Astrophysics Data System (ADS)

    Lodwick, Jeffrey C.

    An anthropometric leg phantom developed at the University of Cincinnati (UC) was used to evaluate the effects that changes in leg position and variation between subjects has on in vivo x-ray fluorescence (XRF) measurements of stable lead in bone. The changes in leg position that were evaluated include changes in source-phantom distance ranging between 0.0 mm and 30.0 mm and phantom rotation over 40 degrees. Source-phantom distance was determined to have a significant effect on XRF measurement results particularly at source-phantom distances greater than 10.0 mm. Rotation of the leg phantom through 40 degrees was determined to have no significant effect on XRF measurement results. Between subject factors that were evaluated include bone calcium content and overlying tissue thickness. Bone calcium content was determined to have a significant effect on XRF measurements when measuring lead in micrograms per gram bone material. However, if measurement results of micrograms of lead per gram calcium (or per gram bone mineral) is used the normalization method makes the change in calcium content not significant. Overlying tissue thickness was determined to have no significant effect on XRF measurement results with tissue thickness ranging between 5.7 and 11.62 mm. The UC leg phantom was modified to include a fibula bone phantom so that the effect that the fibula has on XRF measurement results could be evaluated. The fibula was determined to have no significant effect on XRF measurement results and in the future need not be incorporated into in vivo XRF calibration phantoms. A knee phantom was also developed for purposes of calibrations of in vivo XRF measurement of lead in the patella. XRF measurement results using this phantom were compared to results of XRF measurements made using the plaster-of-Paris (POP) phantoms. A significant difference was observed between the normalized count rates of the two phantom types when either micrograms of lead per gram of bone material or

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

    SciTech Connect

    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

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

    SciTech Connect

    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. Investigation of molecular mechanisms of action of chelating drugs on protein-lipid model membranes by X-ray fluorescence

    SciTech Connect

    Novikova, N. N.; Zheludeva, S. I.; Koval'chuk, M. V.; Stepina, N. D.; Erko, A. I.; Yur'eva, E. A.

    2009-12-15

    Protein-lipid films based on the enzyme alkaline phosphatase were subjected to the action of chelating drugs, which are used for accelerating the removal of heavy metals from the human body, and the elemental composition of the resulting films was investigated. Total-reflection X-ray fluorescence measurements were performed at the Berlin Electron Storage Ring Company for Synchrotron Radiation (BESSY) in Germany. A comparative estimation of the protective effect of four drugs (EDTA, succimer, xydiphone, and mediphon) on membrane-bound enzymes damaged by lead ions was made. The changes in the elemental composition of the protein-lipid films caused by high doses of chelating drugs were investigated. It was shown that state-of-the-art X-ray techniques can, in principle, be used to develop new methods for the in vitro evaluation of the efficiency of drugs, providing differential data on their actions.

  20. Calculation of depth-dependent elemental concentration with X-ray fluorescence using a layered calibration method

    NASA Astrophysics Data System (ADS)

    Gherase, M. R.; Fleming, D. E. B.

    2011-05-01

    Depth-dependent elemental concentration can be assessed using either multiple-angle or confocal X-ray fluorescence (XRF) measurements. This work presents a different approach based on a layered calibration method. The depth-dependent elemental concentration was modeled as multiple layers of uniform elemental concentrations. The unknown elemental concentration in each layer can be calculated using a single-angle XRF measurement, layered calibration data, and a priori knowledge of the concentration behavior as a function of depth. The method was verified using a commercial portable X-ray spectrometer and four-layer stacks of polyester resin discs doped with various concentrations of arsenic. This approach is particularly suitable for quantitative in vivo measurements of arsenic and selenium concentrations in the human skin since minimal ionizing radiation exposure constrains the number of XRF measurements.

  1. [X-ray fluorescence spectrometric determination of high rhenium content in rhenium-tungsten alloys used in traveling wave tube].

    PubMed

    Bao, Sheng-xiang; Wang, Shou-xu; Ma, Li-li; Zhao, Deng-hua; Fan, Rong-kui; Li, Jian

    2005-03-01

    The matrix effect, spectral overlap and background were investigated for X-ray fluorescence (XRF) spectrometric determination of rhenium content according to the analysis requirement of rhenium-tungsten alloys, a key material used in traveling wave tube. The reason for causing the calibration curve nonlinear was explained theoretically when binary ratio technique of XRF was used. Both theoretical and experimental results show that linear calibration curve can be obtained if the curve is plotted by Re% vs. Re Lalpha X-ray intensity instead of binary ratio technique. The method is rapid and accurate and the results obtained in this work are in good agreement with those of chemical analysis. The method has been successfully applied to product quality control. PMID:16013333

  2. Improving limited-projection-angle fluorescence molecular tomography using a co-registered x-ray computed tomography scan

    NASA Astrophysics Data System (ADS)

    Radrich, Karin; Ale, Angelique; Ermolayev, Vladimir; Ntziachristos, Vasilis

    2012-12-01

    We examine the improvement in imaging performance, such as axial resolution and signal localization, when employing limited-projection-angle fluorescence molecular tomography (FMT) together with x-ray computed tomography (XCT) measurements versus stand-alone FMT. For this purpose, we employed living mice, bearing a spontaneous lung tumor model, and imaged them with FMT and XCT under identical geometrical conditions using fluorescent probes for cancer targeting. The XCT data was employed, herein, as structural prior information to guide the FMT reconstruction. Gold standard images were provided by fluorescence images of mouse cryoslices, providing the ground truth in fluorescence bio-distribution. Upon comparison of FMT images versus images reconstructed using hybrid FMT and XCT data, we demonstrate marked improvements in image accuracy. This work relates to currently disseminated FMT systems, using limited projection scans, and can be employed to enhance their performance.

  3. [Energy dispersive x-ray fluorescence spectrometry--a forensic chemistry method for detection of bullet metal residue in gunshot wounds].

    PubMed

    Havel, J; Zelenka, K

    2003-04-01

    The article describes using of energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic method as the tool for detection of metals (gunshot residues--GSR) in connection with gunshot-wounds of persons. PMID:12874887

  4. In-situ Measurements of Colloid Transport and Retention Using Synchroton X-ray Fluorescence

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The physics regarding the retention and mobilization of colloids in saturated and unsaturated conditions remains poorly understood, partially due to the inability to measure colloid concentrations in-situ. In this study, we attached Cd+2 ions to clay colloids, and used synchrotron x-rays to cause th...

  5. POLYMER FILM STANDARDS FOR X-RAY FLUORESCENCE SPECTROMETERS (JOURNAL VERSION)

    EPA Science Inventory

    Sets of thin polymer films were developed to serve as standards for XRF analysis of the following 18 elements in aerosol particle samples: Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, As, Rb, Sr, Zr, Cd, Sb, Ba, and Pb. Each film contains a pair of elements having non-interfering x-ray...

  6. A feasibility study to determine the potential of in vivo detection of gadolinium by x-ray fluorescence (XRF) following gadolinium-based contrast-enhanced MRI.

    PubMed

    Mostafaei, F; McNeill, F E; Chettle, D R; Noseworthy, M D

    2015-01-01

    The feasibility of using a (109)Cd γ-ray induced K x-ray fluorescence (K-XRF) system for the in vivo detection of gadolinium (Gd) in bone has been investigated. The K-XRF bone measurement system employs an array of four detectors, and is normally used for the non-invasive study of bone lead levels. The system was used to measure bone simulating phantoms doped with varying levels of gadolinium and fixed amounts of sodium (Na), chlorine (Cl) and calcium (Ca). The detection limits for bare bone phantoms, using a source of activity 0.17 GBq, were determined to be 3.9 ppm and 6.5 ppm (µg Gd per gram phantom) for the Kα1 and Kα2 Gd x-ray peaks, respectively. This leads to an overall detection limit of 3.3 ppm (µg Gd per gram phantom). Layers of plastic were used to simulate overlying soft tissue and this permitted prediction of a detection limit, using the current strength of our radioisotope source, of 6.1 ppm to 8.6 ppm (µg Gd per gram phantom) for fingers with 2-4 mm of overlying tissue. With a new source of activity 5 GBq, we predict that this system could achieve a detection limit of 4-5.6 µg Gd g(-1) Ca. This is within the range of levels (2-30 µg Gd g(-1) Ca) previously found in the bone of patients receiving Gd based contrast imaging agents. The technique is promising and warrants further investigation. PMID:25501799

  7. Practical Considerations in Trace Element Analysis of Bone by Portable X-ray Fluorescence.

    PubMed

    Byrnes, Jennifer F; Bush, Peter J

    2016-07-01

    Forensic anthropologists are more often turning to nondestructive methods to assist with skeletal analyses, specifically for trace elemental analyses. Portable XRF (pXRF) instruments are versatile and are able to be used in diverse settings or for specimens of a shape and size that cannot be accommodated by laboratory-based instruments. Use of XRF requires knowledge of analysis parameters such as X-ray penetration and exit depth. Analysis depth was determined by examining pure elements through known thicknesses of equine bone slices. Correlation between the element's X-ray emission energy and the depth of reading was observed. Bone surfaces from a small unknown historic cemetery were analyzed before and after sanding of the periosteal surface to observe possible changes in XRF readings based on potential diagenesis. Results validate the pXRF device as a powerful and convenient instrument for nondestructive analysis, while highlighting limitations and considerations for the analysis of osseous materials. PMID:27093090

  8. Absolute Dating of Desert Varnish Using Portable X-Ray Fluorescence: Calibration and Testing

    NASA Astrophysics Data System (ADS)

    Pingitore, N. E.; Lytle, F. W.; Rowley, P. D.; Ferris, D. E.

    2004-12-01

    Desert varnish, also called rock varnish, is a thin biogenic layer of Mn-oxides, Fe-oxides, and clays that coats rock surfaces in arid and semi-arid regions. The mass of these metals in the varnish registers cumulative biologic activity over time and presents a possible dating mechanism, subject to appropriate assumptions and restrictions. We have used a portable x-ray fluorescence (PXRF) unit to measure Mn and Fe in numerous desert varnishes, both in the field and laboratory; the anticipated relationship between age and mass emerges from these data. Our attempts to refine the PXRF technique for absolute dating of desert varnish are confounded by the limited number of "dated" varnishes available to calibrate and test the method. Although there is no current method to directly ascertain the age of desert varnish, our search for "dated" varnishes has yielded three suitable types of test materials: (1) The ages of young basalt flows dated by various K/Ar radiometric techniques represent the maximum age of varnish developed on those surfaces. Such rocks are useful in the time range of perhaps 250,000 to 10,000 years; surface spalling with loss of varnish presents an upper time limit and difficulty in dating Holocene basalts presents a lower limit. Basalt flows typically provide horizontal surfaces that are ideal for PXRF measurements because, as a biogenic process, varnish development even at a single site varies with solar orientation. (2) Petroglyphs are the rock art that native peoples produced by pecking away varnish to expose fresh rock. This process restarts varnish development and the pecked surface gradually repatinates over time. At some locales, certain figures, symbols, and stylistic elements can be associated with an archaeological culture of known antiquity and duration, thus providing an age range for such glyphs. In the desert Southwest and Great Basin of the United States, appropriate glyphs are known from the present to at least 7000 years BP. Many of

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

    NASA Astrophysics Data System (ADS)

    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

  10. Scanning X-ray fluorescent elemental microanalysis with synchrotron radiation in geochemical research

    NASA Astrophysics Data System (ADS)

    Darin, A.; Kalugin, I.; Zolotarev, K.

    2009-04-01

    The traditional XRF analysis with high limits of detection is limited in application for geochemical researches. Use of synchrotron radiation considerably expands its opportunities [1]. Since 1985 in BINP analytical works with syncrotron radiation from storage ring VEPP-3 are carried out. A plenty of methodical and research works with geochemical samples has been executed. The range of energy excitation 15 - 50 keV is now accessible, that allows to determine the following elements in geological samples weight from 1 mg: P, S, Cl, K, Ca, Ti (LD=50 ppm, St.dev.=5 ppm); V, Cr, Mn, Fe, Co, Ni (LD=5 ppm, St.dev.=0.5 ppm); Cu, Zn, Ga, Ge, As, Se (LD=0.5 ppm, St.dev.=0.05 ppm); Br, Rb, Sr, Y, Zr, Nb, Mo (LD=0.1 ppm, St.dev.=0.03 ppm); Ru, Rh, Pd, Ag (LD=0.05 ppm, St.dev.=0.01 ppm); Cd, In, Sn, Sb, Te, I (LD=0.1 ppm, St.dev.=0.03 ppm); Ba, La, Ce, Nd, Sm (LD=1.0 ppm, St.dev.=0.15 ppm); Pb, Bi, Th, U (LD=1 ppm, St.dev.=0.1 ppm). The analysis is carried out in some stages with use various energy of excitation (usually - 15-18, 22 - 25 and 40-45 keV). The first instrument of scanning X-ray fluorescent elemental microanalysis with synchrotron radiation from storage ring VEPP-3 (scan.XRFA-SR) was founded in BINP SB RAS in the 1988 and applied to study the spatial distribution of elements in geological samples [2]. Scan.XRFA-SR was used in paleoclimate reconstructions based on high-resolution sediments and tree-rings analysis [3, 4, 5]. Unique opportunities of XRF SR allow to carry out scanning microanalysis with spatial resolution ~ 10 micron. The set of analyzed elements and range of concentration are determined by selection of energy of excitation and time of measurement in a point. In recent years, has been studied many different geological samples: diamonds, xenolith, ferromanganese nodules, bottom sediments. Studies have demonstrated the unique ability of scanning XRFA-SR: a simultaneous analysis of more than 30 chemical elements with a spatial resolution of 10-50 microns

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

    SciTech Connect

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

    2007-02-12

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  14. Engineering iodine-doped carbon dots as dual-modal probes for fluorescence and X-ray CT imaging

    PubMed Central

    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. PMID:26609232

  15. Fluorescence background subtraction technique for hybrid fluorescence molecular tomography/x-ray computed tomography imaging of a mouse model of early stage lung cancer

    NASA Astrophysics Data System (ADS)

    Ale, Angelique; Ermolayev, Vladimir; Deliolanis, Nikolaos C.; Ntziachristos, Vasilis

    2013-05-01

    The ability to visualize early stage lung cancer is important in the study of biomarkers and targeting agents that could lead to earlier diagnosis. The recent development of hybrid free-space 360-deg fluorescence molecular tomography (FMT) and x-ray computed tomography (XCT) imaging yields a superior optical imaging modality for three-dimensional small animal fluorescence imaging over stand-alone optical systems. Imaging accuracy was improved by using XCT information in the fluorescence reconstruction method. Despite this progress, the detection sensitivity of targeted fluorescence agents remains limited by nonspecific background accumulation of the fluorochrome employed, which complicates early detection of murine cancers. Therefore we examine whether x-ray CT information and bulk fluorescence detection can be combined to increase detection sensitivity. Correspondingly, we research the performance of a data-driven fluorescence background estimator employed for subtraction of background fluorescence from acquisition data. Using mice containing known fluorochromes ex vivo, we demonstrate the reduction of background signals from reconstructed images and sensitivity improvements. Finally, by applying the method to in vivo data from K-ras transgenic mice developing lung cancer, we find small tumors at an early stage compared with reconstructions performed using raw data. We conclude with the benefits of employing fluorescence subtraction in hybrid FMT-XCT for early detection studies.

  16. Gadolinium Deposition in Nephrogenic Systemic Fibrosis: An Examination of Tissue using Synchrotron X-ray Fluorescence Spectroscopy

    SciTech Connect

    High, W.; Ranville, J; Brown, M; Punshon, T; Lanzirotti, A; Jackson, B

    2010-01-01

    Nephrogenic systemic fibrosis is a fibrosing disorder associated with gadolinium (Gd)-based contrast agents dosed during renal insufficiency. In two patients, Gd deposition in tissue affected by nephrogenic systemic fibrosis was quantified using inductively coupled plasma mass spectrometry. The presence of Gd was confirmed and mapped using synchrotron x-ray fluorescence spectroscopy. Affected skin and soft tissue from the lower extremity demonstrated 89 and 209 ppm ({micro}g/g, dry weight, formalin fixed) in cases 1 and 2, respectively. In case 2, the same skin and soft tissue was retested after paraffin embedding, with the fat content removed by xylene washes, and this resulted in a measured value of 189 ppm ({micro}g/g, dry weight, paraffin embedded). Synchrotron x-ray fluorescence spectroscopy confirmed Gd in the affected tissue of both cases, and provided high-sensitivity and high-resolution spatial mapping of Gd deposition. A gradient of Gd deposition in tissue correlated with fibrosis and cellularity. Gd deposited in periadnexal locations within the skin, including hair and eccrine ducts, where it colocalized to areas of high calcium and zinc content. Because of the difficulty in obtaining synchrotron x-ray fluorescence spectroscopy scans, tissue from only two patients were mapped. A single control with kidney disease and gadolinium-based contrast agent exposure did not contain Gd. Gd content on a gravimetric basis was impacted by processing that removed fat and altered the dry weight of the specimens. Gradients of Gd deposition in tissue corresponded to fibrosis and cellularity. Adnexal deposition of Gd correlated with areas of high calcium and zinc content.

  17. A portable micro-X-ray fluorescence spectrometer with polycapillary optics and vacuum chamber for archaeometric and other applications

    NASA Astrophysics Data System (ADS)

    Buzanich, G.; Wobrauschek, P.; Streli, C.; Markowicz, A.; Wegrzynek, D.; Chinea-Cano, E.; Bamford, S.

    2007-11-01

    A portable focused-beam XRF spectrometer was designed, constructed, and manufactured. The spectrometer allows to detect and perform analysis of chemical elements from Na upwards. The system is equipped with a compact vacuum chamber to reduce absorption of both the excitation and the fluorescence radiation in air. A low power Pd-anode tube operated up to 50 kV and 1 mA with a point focus of 400 μm is used as excitation source. A polycapillary lens with a spot size of about 160 μm, or a collimator with a 1 mm inner diameter can be used alternatively for either focusing or collimating the primary beam. The fluorescence radiation is collected by an Si drift detector with an active area of 10 mm 2 and equipped with an 8 μm Be entrance window. A compact vacuum chamber was designed to house the X-ray beam optics and the detector snout. The chamber is attached to the X-ray tube and can be pumped down to 0.1 mbar. A Kapton™ window of 7.5 μm thickness allows to locate the investigated spot at about 1-2 mm distance outside of the chamber, thus minimizing absorption losses in the excitation and X-ray fluorescence radiation paths. Two lasers pointers are mounted inside the chamber. The laser beams cross at a point outside the chamber in front of the entrance window and coincide with the focal spot of the polycapillary. This paper reports some preliminary results obtained from an in situ analysis of bronze samples as well as a comparison of these data with those given by other laboratory spectrometers and the reference values provided by the Italian bronze foundry Venturi Arte Bologna, Italy.

  18. The study of in vivo x-ray fluorescence (XRF) technique for gadolinium (Gd) measurements in human bone

    NASA Astrophysics Data System (ADS)

    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.

  19. Crystallization and preliminary X-ray characterization of the genetically encoded fluorescent calcium indicator protein GCaMP2

    SciTech Connect

    Rodríguez Guilbe, María M.; Alfaro Malavé, Elisa C.; Akerboom, Jasper; Marvin, Jonathan S.; Looger, Loren L.; Schreiter, Eric R.

    2008-07-01

    The genetically encoded fluorescent calcium-indicator protein GCaMP2 was crystallized in the calcium-saturated form. X-ray diffraction data were collected to 2.0 Å resolution and the structure was solved by molecular replacement. Fluorescent proteins and their engineered variants have played an important role in the study of biology. The genetically encoded calcium-indicator protein GCaMP2 comprises a circularly permuted fluorescent protein coupled to the calcium-binding protein calmodulin and a calmodulin target peptide, M13, derived from the intracellular calmodulin target myosin light-chain kinase and has been used to image calcium transients in vivo. To aid rational efforts to engineer improved variants of GCaMP2, this protein was crystallized in the calcium-saturated form. X-ray diffraction data were collected to 2.0 Å resolution. The crystals belong to space group C2, with unit-cell parameters a = 126.1, b = 47.1, c = 68.8 Å, β = 100.5° and one GCaMP2 molecule in the asymmetric unit. The structure was phased by molecular replacement and refinement is currently under way.

  20. The study of chemical composition and elemental mappings of colored over-glaze porcelain fired in Qing Dynasty by micro-X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    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.