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Sample records for handheld x-ray fluorescence

  1. Algorithms for a hand-held miniature x-ray fluorescence analytical instrument

    Energy Technology Data Exchange (ETDEWEB)

    Elam, W.T.; Newman, D.; Ziemba, F. [and others

    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.

  2. Novel handheld x-ray fluorescence spectrometer for routine testing for the presence of lead

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    Miller, Gillian Zaharias; Harris, Zoe E

    2015-01-01

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

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

    Science.gov (United States)

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

    2011-12-01

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

  5. Calibration of handheld X-ray fluorescence (XRF) equipment for optimum determination of elemental concentrations in sediment samples.

    Science.gov (United States)

    Mejía-Piña, K Gabriela; Huerta-Diaz, Miguel Angel; González-Yajimovich, O

    2016-12-01

    Handheld X-ray fluorescence spectrometers (XRFs) represent a more practical, efficient and economic tool to determine the elemental composition of solid inorganic and organic samples than conventional analytical techniques. The objective of this work was to demonstrate that handheld XRFs could be a precise, accurate and reliable tool to analyze up to 27 different elements. This objective was accomplished through the optimization of an empirical calibration curve that, in addition to include certified reference materials (CRM), it also introduced new approaches, such as the use of solid CRM mixtures and combinations of organic and inorganic matrices. These approaches significantly increased the number of calibration points and eliminated hiatuses in the calibration curve. Several factors were evaluated before construction of the calibration curve: incidence time of the X-ray beam, type of film through which the X-ray beams reach the samples, container type, minimum sample volume and sample moisture content. Results show that single elements can be analyzed with variable exposure times or, alternatively, multielemental analyses can be carried out with a constant exposure time (180s). Costs can be reduced by using Ziploc ® bags as sample containers, but the number of measurable elements drops from 27 to 21, while the possibility of contamination increases. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Non-destructive measurement of calcium and potassium in apple and pear using handheld x-ray fluorescence

    Directory of Open Access Journals (Sweden)

    Lee A Kalcsits

    2016-04-01

    Full Text Available Calcium and potassium are essential for cell signalling, ion homeostasis and cell wall strength in plants. Unlike nutrients such as nitrogen and potassium, calcium is immobile in plants. Localized calcium deficiencies result in agricultural losses; particularly for fleshy horticultural crops in which elemental imbalances in fruit contribute to the development of physiological disorders such as bitter pit in apple and cork spot in pear. Currently, elemental analysis of plant tissue is destructive, time consuming and costly. This is a limitation for nutrition studies related to calcium in plants. Handheld portable x-ray fluorescence (XRF can be used to non-destructively measure elemental concentrations. The main objective was to test if handheld XRF can be used for semi-quantitative calcium and potassium analysis of in-tact apple and pear. Semi-quantitative measurements for individual fruit were compared to results obtained from traditional lab analysis. Here, we observed significant correlations between handheld XRF measurements of calcium and potassium and concentrations determined using MP-AES lab analysis. Pearson correlation coefficients ranged from 0.73 and 0.97. Furthermore, measuring apple and pear using handheld XRF identified spatial variability in calcium and potassium concentrations on the surface of individual fruit. This variability may contribute to the development of localized nutritional imbalances. This highlights the importance of understanding spatial and temporal variability in elemental concentrations in plant tissue. Handheld XRF is a relatively high-throughput approach for measuring calcium and potassium in plant tissue. It can be used in conjunction with traditional lab analysis to better understand spatial and temporal patterns in calcium and potassium uptake and distribution within an organ, plant or across the landscape.

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

    Directory of Open Access Journals (Sweden)

    Madalena Kozachuk

    2016-05-01

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

  8. Tracing euxinia by molybdenum concentrations in sediments using handheld X-ray fluorescence spectroscopy (HHXRF)

    DEFF Research Database (Denmark)

    Dahl, Tais W.; Ruhl, Micha; Hammarlund, Emma U.

    2013-01-01

    sigma) after a daily calibration to samples covering a range of Mo concentrations from 0 to >30 ppm. Hand-held XRF equipment also allows Mo measurements directly on fresh rock surfaces, both in the field and under laboratory conditions. Rock-samples from a Cambrian drill core closely match ICPMS...

  9. Evaluating Handheld X-Ray Fluorescence (XRF) Technology in Planetary Exploration: Demonstrating Instrument Stability and Understanding Analytical Constraints and Limits for Basaltic Rocks

    Science.gov (United States)

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

    2012-01-01

    While large-footprint X-ray fluorescence (XRF) instruments are reliable providers of elemental information about geologic samples, handheld XRF instruments are currently being developed that enable the collection of geochemical data in the field in short time periods (approx.60 seconds) [1]. These detectors are lightweight (1.3kg) and can provide elemental abundances of major rock forming elements heavier than Na. While handheld XRF detectors were originally developed for use in mining, we are working with commercially available instruments as prototypes to explore how portable XRF technology may enable planetary field science [2,3,4]. If an astronaut or robotic explorer visited another planetary surface, the ability to obtain and evaluate geochemical data in real-time would be invaluable, especially in the high-grading of samples to determine which should be returned to Earth. We present our results on the evaluation of handheld XRF technology as a geochemical tool in the context of planetary exploration.

  10. User certification of hand-held x-ray tube based analytical fluorescent devices in a canadian context

    Energy Technology Data Exchange (ETDEWEB)

    Maharaj, H.P. [Department of Health, Consumer and Clinical Radiation Protection Bureau, Ottawa, Ontario (Canada)

    2005-07-01

    Safety education aims to reduce personal injury and improve well being. This health promotion principle is applied in the case of hand-held open beam x-ray tube based analytical x-ray devices. Such devices not only are light weight and portable, but also present high radiation exposure levels at the beam exit port and potentially can be used in a variety of industrial applications for determination of material composition. There is much potential for radiation risks to occur with resultant adverse effects if such devices are not used by trained individuals within controlled environments. A level of radiation safety knowledge and understanding of the device design, construction and performance characteristics appear warranted. To reduce radiation risks, user certification at a federal level was introduced in 2004 based on International Standards Organization 20807, since that standard comprises elements commensurate with risk reduction strategies. Within these contexts, a federally certified user is deemed to have acquired a level of safety knowledge and skills to facilitate safe use of the device. Certification, however, does not absolve the holder from obligations of compliance with applicable provincial, territorial or federal laws respecting device operation. The union of federal certification and applicable legislative mandated operational criteria reduces radiation risks overall. (author)

  11. X-ray fluorescence holography

    CERN Document Server

    Hayashi, K; Takahashi, Y

    2003-01-01

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

  12. Elemental Analysis of Bone, Teeth, Horn and Antler in Different Animal Species Using Non-Invasive Handheld X-Ray Fluorescence.

    Directory of Open Access Journals (Sweden)

    Kittisak Buddhachat

    Full Text Available Mineralized tissues accumulate elements that play crucial roles in animal health. Although elemental content of bone, blood and teeth of human and some animal species have been characterized, data for many others are lacking, as well as species comparisons. Here we describe the distribution of elements in horn (Bovidae, antler (Cervidae, teeth and bone (humerus across a number of species determined by handheld X-ray fluorescence (XRF to better understand differences and potential biological relevance. A difference in elemental profiles between horns and antlers was observed, possibly due to the outer layer of horns being comprised of keratin, whereas antlers are true bone. Species differences in tissue elemental content may be intrinsic, but also related to feeding habits that contribute to mineral accumulation, particularly for toxic heavy metals. One significant finding was a higher level of iron (Fe in the humerus bone of elephants compared to other species. This may be an adaptation of the hematopoietic system by distributing Fe throughout the bone rather than the marrow, as elephant humerus lacks a marrow cavity. We also conducted discriminant analysis and found XRF was capable of distinguishing samples from different species, with humerus bone being the best source for species discrimination. For example, we found a 79.2% correct prediction and success rate of 80% for classification between human and non-human humerus bone. These findings show that handheld XRF can serve as an effective tool for the biological study of elemental composition in mineralized tissue samples and may have a forensic application.

  13. Preliminary validation of handheld X-ray fluorescence spectrometry: distinguishing osseous and dental tissue from nonbone material of similar chemical composition.

    Science.gov (United States)

    Zimmerman, Heather A; Schultz, John J; Sigman, Michael E

    2015-03-01

    One of the tasks of a forensic anthropologist is to sort human bone fragments from other materials, which can be difficult when dealing with highly fragmented and taphonomically modified material. The purpose of this research is to develop a method using handheld X-ray fluorescence (HHXRF) spectrometry to distinguish human and nonhuman bone/teeth from nonbone materials of similar chemical composition using multivariate statistical analyses. The sample materials were derived primarily from previous studies: human bone and teeth, nonhuman bone, nonbiological materials, nonbone biological materials, and taphonomically modified materials. The testing included two phases, testing both the reliability of the instrument and the accuracy of the technique. The results indicate that osseous and dental tissue can be distinguished from nonbone material of similar chemical composition with a high degree of accuracy (94%). While it was not possible to discriminate rock apatite and synthetic hydroxyapatite from bone/teeth, this technique successfully discriminated ivory and octocoral. © 2015 American Academy of Forensic Sciences.

  14. An assessment of a handheld X-ray fluorescence instrument for use in exploration and development with an emphasis on REEs and related specialty metals

    Science.gov (United States)

    Simandl, G. J.; Stone, R. S.; Paradis, S.; Fajber, R.; Reid, H. M.; Grattan, K.

    2014-12-01

    Handheld (portable) X-ray fluorescence (pXRF) instruments are designed for use in the exploration for base metals, precious metals, and specialty metals (e.g. rare earth elements (REE), Ta, and Nb) and allow rapid decision-making directly in the field. This paper evaluates the technical merits and limitations of pXRF technology in the exploration for specialty metals using data generated from the analysis of three geochemical standards and a silica blank: Standard Reference Material NIST 2780 from the National Institute of Standards and Technology, Gaithersburg; the Certified Reference Material "TRLK" Rare Earth Ore "CGL 124" from the Mongolia Central Geological Laboratory; the Reference Niobium Ore OKA-1 (CANMET); and a silica blank described as Si (IV) oxide (99.8 % on metal basis) from Alpha Aesar (Ward Hill, MA, USA). The data was acquired over a period of nearly 2 years as a by-product of several distinct specialty metal-related projects using the same pXRF instrument and the same settings. Instrumental analytical accuracy was determined using the percent difference (%diff) between the average concentrations of the pXRF instrument readings and the reported certified values of the standard. Percent relative standard deviation (%RSD) was used as a measure of precision. Smaller %diff and %RSD indicate more accurate and precise data, and the accuracy and precision of the pXRF depended strongly on the elemental concentrations in the standards used. Box and whisker diagrams were used to illustrate characteristics of pXRF data sets (mean, lower and upper quartiles, and range) corresponding to individual standards. The bias of the pXRF determinations (under/overestimation) relative to certified values of individual standards are also depicted on these diagrams. This study indicates that the pXRF was capable of producing readings for Si, K, Al, Fe, Ca, Ti, Pb, Zn, Sr, Ag, Cd, Th, Sb, P, S, Mo, Mn, Mg, As, Nb, Rb, La, Ce, Pr, Nd, and Y within 10 %RSD of the reported

  15. The Use of Handheld X-Ray Fluorescence (XRF) Technology in Unraveling the Eruptive History of the San Francisco Volcanic Field, Arizona

    Science.gov (United States)

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

    2012-01-01

    While traditional geologic mapping includes the examination of structural relationships between rock units in the field, more advanced technology now enables us to simultaneously collect and combine analytical datasets with field observations. Information about tectonomagmatic processes can be gleaned from these combined data products. Historically, construction of multi-layered field maps that include sample data has been accomplished serially (first map and collect samples, analyze samples, combine data, and finally, readjust maps and conclusions about geologic history based on combined data sets). New instruments that can be used in the field, such as a handheld xray fluorescence (XRF) unit, are now available. Targeted use of such instruments enables geologists to collect preliminary geochemical data while in the field so that they can optimize scientific data return from each field traverse. Our study tests the application of this technology and projects the benefits gained by real-time geochemical data in the field. The integrated data set produces a richer geologic map and facilitates a stronger contextual picture for field geologists when collecting field observations and samples for future laboratory work. Real-time geochemical data on samples also provide valuable insight regarding sampling decisions by the field geologist

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

    Energy Technology Data Exchange (ETDEWEB)

    Gherase, Mihai R., E-mail: mgherase@csufresno.edu; Vargas, Andres Felipe

    2017-03-15

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

  17. Review of X-ray Tomography and X-ray Fluorescence Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Shear, Trevor A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-03-16

    This literature review will focus on both laboratory and synchrotron based X-ray tomography of materials and highlight the inner workings of these instruments. X-ray fluorescence spectroscopy will also be reviewed and applications of the tandem use of these techniques will be explored. The real world application of these techniques during the internship will also be discussed.

  18. Advanced in X-ray fluorescence holography

    CERN Document Server

    Hayashi, K

    2002-01-01

    X-ray fluorescence holography (XFH) can resolve 'phase problem' in crystal diffraction and therefore it provides 3D atomic images around specific elements. Since first demonstration of the XFH in 1996, view of atoms has been improved rapidly with the refinement of the hologram data collection method. The present performance of the XFH makes it possible to apply to impurity, thin film and quasicrystal, and opens a way to practical tool for determination of local structure. In this paper, theory including solutions for twin image problem, advanced experimental systems and application to Si sub 0 sub . sub 9 sub 9 sub 9 Ge sub 0 sub . sub 0 sub 0 sub 1 are discussed. (author)

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

    Indian Academy of Sciences (India)

    in rainwater are, inductively coupled plasma-mass spectrometry (ICPMS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), atomic absorption spectrom- etry (AAS), X-ray fluorescence (XRF), total reflection X-ray fluorescence (TXRF), neu- tron activation analysis (NAA), electroanalytical techniques, etc.

  20. Milli X-Ray Fluorescence Spectrometer

    Data.gov (United States)

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

  1. Use of X-Ray Fluorescence Spectrometry to Determine Trace ...

    African Journals Online (AJOL)

    This paper deals with application of X-ray fluorescence spectrometry for the detection of trace elements in graphic. An X-ray spectrometer was constructed and used to carry out measurements on graphite spheres impregnated with different chemical elements. The intensities of the lines of these trace elements, as function of ...

  2. X-ray fluorescence in investigations of archaeological finds

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-15

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

  3. [Development of X-ray excited fluorescence spectrometer].

    Science.gov (United States)

    Ni, Chen; Gu, Mu; Di, Wang; Cao, Dun-Hua; Liu, Xiao-Lin; Huang, Shi-Ming

    2009-08-01

    An X-ray excited fluorescence spectrometer was developed with an X-ray tube and a spectrometer. The X-ray tube, spectrometer, autocontrol method and data processing selected were roundly evaluated. The wavelength and detecting efficiency of the apparatus were calibrated with the mercury and tungsten bromine standard lamps, and the X-ray excited emission spectra of BaF2, Cs I (Tl) crystals were measured. The results indicate that the apparatus has advantages of good wavelength resolution, high stability, easy to operation and good radioprotection. It is a wery effective tool for exploration of new scintillation materials.

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

    Science.gov (United States)

    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.

  5. FLUORESCENT X-RAY IMAGING WITH PINHOLE CAMERA

    Directory of Open Access Journals (Sweden)

    Yu. I. Dudchik

    2016-01-01

    Full Text Available Pinhole camera is one of X-ray optics devices. The pinhole camera is used for obtaining the image of synchrotron and laboratory sources, and also as a lens in a method of X-ray fluorescent microscopy. This method allows to obtain information on a spatial distribution of various chemical elements to the areas of several square centimeters with spatial resolution at the level of 50–100 μm. As a rule energy-dispersive two-dimensional CCD cameras are used for imaging. Such cameras are expensive devices and have low sensitivity for X-rays with energy of photons higher than 8 keV. Therefore it is perspective to use for X-ray fluorescent microscopy more effective CCD cameras with a scintillator layer. The purpose of this work consists in development of the device for imaging with secondary fluorescent X-rays by using pinhole as a lens and CCD camera for registration of the X-ray image. The device for obtaining the image of objects in secondary X-rays is developed. The device consists of an X-ray tube, pinhole and CCD camera. The object of research was irradiated with radiation from the X-ray tube and emits secondary X-rays. 100-microns pinhole was used for formation of the image of the object at an entrance window of the CCD camera. Images of a number of the iron springs differing in the sizes are received. It is established that the spatial resolution of the device is about 200 μm at an exposition of 60 s. It is possible to improve permission of the device by increasing in an exposition, optimization imaging conditions and reduction of the pinhole size. 

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1978-06-01

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

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

    Science.gov (United States)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2010-01-01

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

  9. Research Note: Energy dispersive x-ray fluorescence analysis ...

    African Journals Online (AJOL)

    Energy Dispersive X-Ray fluorescence (EDXRF) technique for the analysis of geological, biological and environmental samples is described. The technique has been applied in the analysis of 10 (geological, biological, environmental) standard reference materials. The accuracy and precision of the technique were attested ...

  10. X-ray fluorescence spectroscopic determination of heavy metals and ...

    African Journals Online (AJOL)

    Purpose: To determine the heavy metal and trace element composition of the powdered aerial parts of Origanum sipyleum L. and its water extract. Methods: The heavy metal and trace elements content of the powdered plant material and 2 % aqueous extract were evaluated by x-ray fluorescence spectroscopy with silicon ...

  11. Application of total reflection x-ray fluorescence (TXRF) technique ...

    African Journals Online (AJOL)

    Nigerian crude oils from eight oil wells have been analysed for the following trace elements: Ni, Cr, Mn, V, Fe, Zn. Pb, Cu, Co and S using total Reflection X-ray Fluorescence (TXRF) analytical method. Concentrations of these elements were found to range from 0.002 – 1.420 ppm. Results showed that Fe was the most ...

  12. Basic theory and methods of X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Duimakaev, S.I.; Shpolyansky, A.Y.; Duimakaeva, T.G.; Losev, V.N. (Rostovskij-na-Donu Gosudarstvennyj Univ. (USSR)); Vershinina, N.V. (Rostov Inst. of Railway Transport Engineers, Rostov-na-Don (USSR)); Tsvetyansky, A.L. (NPO ' Soyuztsvetmetavtomatika' , Rostov-na-Don (USSR))

    1989-09-01

    The Soviet analysts' major advances in both theory and application of X-ray fluorescence (XRF) analysis are reviewed. The focus is on issues concerning XRF analysis of heterogeneous samples, a theoretical account of interelement effects, and employment of scattered radiation as the internal standard. (orig.).

  13. X-ray fluorescence spectroscopic determination of heavy metals and ...

    African Journals Online (AJOL)

    Purpose: To determine the heavy metal and trace element composition of the powdered aerial parts of. Origanum sipyleum L. and its water extract. Methods: The heavy metal and trace elements content of the powdered plant material and 2 % aqueous extract were evaluated by x-ray fluorescence spectroscopy with silicon ...

  14. Synchrotron-based X-ray fluorescence, imaging and elemental ...

    Indian Academy of Sciences (India)

    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. Keywords. X-ray fluorescence; synchrotron-based excitation; imaging; elemental mapping; biological samples. PACS Nos 78.70.En; 29.20.dk; 87.59.

  15. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    , Ca, Mn, Ti, Cu, Mo, Fe, Zn, Ni, Re, Eu and Pb using Energy Dispersive X-ray fluorescence (ED-XRF) spectrometry, following standard procedures. The results showed varying amounts of the studied elements in the samples from the two ...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-08-09

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-03-21

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

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

    Science.gov (United States)

    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%.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-08-31

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

  20. Proton-induced x-ray fluorescence CT imaging.

    Science.gov (United States)

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

    2015-02-01

    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. 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(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. A linear relationship between gold pXRF and gold concentration was observed in both experimental and MC simulation data (R(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. Proton-induced x-ray fluorescence CT imaging of 3%-5% gold solutions in a small animal sized water phantom has been demonstrated

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-04-15

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

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

    Science.gov (United States)

    Notis, Michael; Newbury, Brian; Stephenson, Bruce; Stephenson, G. Brian

    2013-04-01

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

  4. The Mapping X-Ray Fluorescence Spectrometer (mapx)

    Science.gov (United States)

    Blake, D. F.; Sarrazin, P.; Bristow, T.; Downs, R. T.; Gailhanou, M.; Marchis, F.; Ming, D. W.; Morris, R. V.; Sole, V. A.; Thompson, K.; Walter, P.; Wilson, M.; Yen, A. S.; Webb, S.

    2016-12-01

    MapX will provide elemental imaging at ≤100 µm spatial resolution over 2.5 X 2.5 cm 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 α-particles / γ-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 µm and quantitative XRF spectra from Regions of Interest (ROI) 2 cm ≤ x ≤ 100 µm. 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. [1] Schoonjans, T. et al.(2012). Spectrachim. Acta Part B, 70, 10-23. [2] Agostinelli, S. et al. (2003). Nucl. Instr. and Methods in Phys. Research A, 506, 250-303. [3] V.A. Solé et al. (2007). Spectrochim. Acta Part B, 62, 63-68.

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

    Science.gov (United States)

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

    2017-03-16

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

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Grodzins, Lee; Niland, John

    2002-05-23

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-11

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

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

    Science.gov (United States)

    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.

  10. Effect of the amount of battery charge on tube voltage in different hand-held dental x-ray systems

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Eun Kyung [Dankook University College of Dentistry, Cheonan (Korea, Republic of)

    2012-03-15

    Hand-held dental x-ray system is a self contained x-ray machine designed to perform intraoral radiography with one or two hands. The issue about its usage as general dental radiography is still in dispute. The aim of the present study was to assess the relationship between the amount of battery charge and the tube voltage in different hand-held dental x-ray systems. Seven hand-held dental x-ray units were used for the study. Tube voltage was measured with Unfors ThinX RAD (Unfors Instruments AB, Billdal, Sweden) for 3 consecutive exposures at the different amount of battery charge of each unit. The average and the deviation percentage of measured kV from indicated kV of each unit were calculated. Tube voltage of only 1 unit was 70 kV (indicated by manufacturer) and those of the others were 60 kV. Tube voltage deviation percentage from the indicated kV at the fully charged battery was from 2.5% to -5.5% and from -0.8% to -10.0% at the lowest charged battery. Tube voltages of all units decreased as the residual amount of the battery charge decreased. It is suggested that the performance test for hand-held x-ray system should be performed for the minimum residual charged battery as well as the full charged one. Persistent battery charging is suggested to maintain the proper tube voltage of the hand-held portable x-ray system.

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

    Data.gov (United States)

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

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

    Data.gov (United States)

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

  13. X-ray fluorescence spectrometry and related techniques an introduction

    CERN Document Server

    Margui, Eva

    2013-01-01

    X-ray fluorescence spectrometry (XRF) is a well-established analytical technique for qualitative and quantitative elemental analysis of a wide variety of routine quality control and research samples. Among its many desirable features, it delivers true multi-element character analysis, acceptable speed and economy, easy of automation, and the capacity to analyze solid samples. This remarkable contribution to this field provides a comprehensive and up-to-date account of basic principles, recent developments, instrumentation, sample preparation procedures, and applications of XRF analysis. If you are a professional in materials science, analytic chemistry, or physics, you will benefit from not only the review of basics, but also the newly developed technologies with XRF. Those recent technological advances, including the design of low-power micro- focus tubes and novel X-ray optics and detectors, have made it possible to extend XRF to the analysis of low-Z elements and to obtain 2D or 3D information on a microme...

  14. Simulation and application of micro X-ray fluorescence based on an ellipsoidal capillary

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jing; Li, Yude; Wang, Xingyi; Zhang, Xiaoyun; Lin, Xiaoyan, E-mail: yangjing_928@126.com

    2017-06-15

    Highlights: • A micro X-ray fluorescence setup based on an ellipsoidal capillary was presented. • The optimal parameters of ellipsoidal capillary were designed. • The 2D mapping image of biological sample was obtained. - Abstract: A micro X-ray fluorescence setup was presented, based on an ellipsoidal capillary and a traditional laboratorial X-ray source. Using Ray-tracing principle, we have simulated the transmission path of X-ray beam in the ellipsoidal capillary and designed the optimal parameters of the ellipsoidal capillary for the micro X-ray fluorescence setup. We demonstrate that ellipsoidal capillary is well suited as condenser for the micro X-ray fluorescence based on traditional laboratorial X-ray source. Furthermore, we obtain the 2D mapping image of the leaf blade sample by using the ellipsoidal capillary we designed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-01-01

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

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

    CERN Document Server

    Haschke, Michael

    2014-01-01

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

  17. X-ray microbeam fluorescence and strain measurements during electromigration

    Science.gov (United States)

    Kao, Hsien-Kang (Michael)

    2000-10-01

    Electromigration, atom diffusion caused by an electric current, has long been a matter of concern to the microelectronic industry because it causes failures in thin film interconnects. In industrial practice, a small amount of Cu (0.25 at.%-2 at.%) is alloyed into Al interconnects since Cu is found to inhibit the failure in interconnects caused by electromigration. The beneficial effect of Cu is not fully understood. The available evidence suggests that the Cu is usually swept away from an area by electromigration before fast Al diffusion leads to appreciable damage in the interconnect. Since grain boundary diffusion is the dominant diffusion mechanism at the relatively low temperatures at which most microelectronic devices are used, and since Cu has very low solid solubility in Al at operating temperatures, Cu segregated into the grain boundaries must reduce the electromigration flux of Al along these dominant paths in order to produce the observed electromigration lifetime improvement. Because of the critical role of Cu in Al(Cu), it is essential to obtain information on the motion and distribution of solute Cu atoms during electromigration. The goal of this research was to obtain for the first time, simultaneously and in real time, spatially resolved information on chemical composition and equal-biaxial stress in polycrystalline Al(Cu) thin film interconnects during electromigration testing. Polychromatic x-ray microbeams from a synchrotron were used. A novel x-ray microbeam instrumentation, developed for this purpose, uses tapered glass capillaries to obtain micron-scale spatial resolution. Two energy dispersive solid state detectors were used to measure simultaneously both solute Cu composition and local strain. Results of Cu concentration mapping showed that the solute Cu concentration as dilute as 500 PPM in the SiO2 passivated Al(Cu) interconnects could be detected through Cu K, fluorescence generated by the incident white x-ray. Time evolution of solute Cu

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

    African Journals Online (AJOL)

    A robust computer program to simulate X-ray fluorescence (XRF) system and particularly applied to the total reflection mode is presented in this paper. The simulation of the different stages involved in x-ray fluorescence emissions was carried out by writing a suite of computer programs using FORTRAN programming ...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-15

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

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

    Science.gov (United States)

    Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

    2016-11-01

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

  2. Portable energy-dispersive X-ray fluorescence equipment for the ...

    Indian Academy of Sciences (India)

    Abstract. Energy-dispersive X-ray fluorescence (EDXRF) especially in its portable version, gen- erally characterized by a small X-ray tube and a Si-PIN or Si-drift detector is particularly useful to analyse works of art. EDXRF technique is nondestructive, noninvasive and multielemental. A variety of works, such as paintings of ...

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

    Indian Academy of Sciences (India)

    X-ray fluorescence (EDXRF) system was developed to analyse alloys by exposing them directly under the tube bremsstrahlung and also under monochromatic X-rays obtained from secondary targets. In both the cases, no standard sample is required. Using the above principle, some archaeological objects were analysed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-04-15

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

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

    Indian Academy of Sciences (India)

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

  6. Detecting Metallic Primary Explosives with a Portable X-ray Fluorescence Spectrometer

    National Research Council Canada - National Science Library

    Hewitt, Alan D

    1997-01-01

    X-ray fluorescence spectrometry (XRF) analysis is a practical means of performing in-situ screening to establish the presence of high concentrations (>0.1% or 1000 ppm) of lead (Pb) and/or mercury (Hg...

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

    National Research Council Canada - National Science Library

    Becker, Andrew

    2008-01-01

    This report describes the application of an X-ray Fluorescence (XRF) instrument to determine the composition of wear debris collected from helicopter magnetic chip detectors and oil filters. The Twin-X XRF...

  8. Multi-pinhole fluorescent x-ray computed tomography for molecular imaging

    National Research Council Canada - National Science Library

    Tenta Sasaya; Naoki Sunaguchi; Kazuyuki Hyodo; Tsutomu Zeniya; Tetsuya Yuasa

    2017-01-01

    We propose a multi-pinhole fluorescent x-ray computed tomography (mp-FXCT) technique for preclinical molecular imaging that can provide the complete data necessary to produce 3-D tomographic images during anaesthesia...

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

    DEFF Research Database (Denmark)

    Christensen, Leif Højslet; Heydorn, Kaj

    1985-01-01

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

  10. LCLS in—photon out: fluorescence measurement of neon using soft x-rays

    Science.gov (United States)

    Obaid, Razib; Buth, Christian; Dakovski, Georgi L.; Beerwerth, Randolf; Holmes, Michael; Aldrich, Jeff; Lin, Ming-Fu; Minitti, Michael; Osipov, Timur; Schlotter, William; Cederbaum, Lorenz S.; Fritzsche, Stephan; Berrah, Nora

    2018-02-01

    We measured the fluorescence photon yield of neon upon soft x-ray ionization (∼1200 eV) from the x-ray free-electron laser at Linac Coherent Light Source, and demonstrated the usage of a grazing incidence spectrometer with a variable line spacing grating to perform x-ray fluorescence spectroscopy on a gas phase system. Our measurements also allowed us to estimate the focal size of the beam from the theoretical description developed, in terms of the rate equation approximation accounting for photoionization shake off of neutral neon and double auger decay of single core holes.

  11. LCLS in - photon out: fluorescence measurement of neon using soft x-rays

    OpenAIRE

    Obaid, Razib; Buth, Christian; Dakovski, Georgi L.; Beerwerth, Randolf; Holmes, Michael; Aldrich, Jeff; Lin, Ming-Fu; Minitti, Michael; Osipov, Timur; Schlotter, William; Cederbaum, Lorenz S.; Fritzsche, Stephan; Berrah, Nora

    2017-01-01

    We measured the fluorescence photon yield of neon upon soft x-ray ionization (~1200 eV) from the x-ray free electron laser at Linac Coherent Light Source, and demonstrated the usage of a grazing incidence spectrometer with a variable linespacing grating to perform x-ray fluorescence spectroscopy on a gas phase system. Our measurements also allowed us to estimate the focal size of the beam from the theoretical description developed, in terms of the rate equation approximation accounting for ph...

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

    Directory of Open Access Journals (Sweden)

    Okuyama, Fumio

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Worley, Christopher Gordon [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-03-04

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

  14. A microfocus X-ray fluorescence beamline at Indus-2 synchrotron radiation facility.

    Science.gov (United States)

    Tiwari, M K; Gupta, P; Sinha, A K; Kane, S R; Singh, A K; Garg, S R; Garg, C K; Lodha, G S; Deb, S K

    2013-03-01

    A microfocus X-ray fluorescence spectroscopy beamline (BL-16) at the Indian synchrotron radiation facility Indus-2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X-ray fluorescence mapping, X-ray microspectroscopy and total-external-reflection fluorescence characterization. The beamline is installed on a bending-magnet source with a working X-ray energy range of 4-20 keV, enabling it to excite K-edges of all elements from S to Nb and L-edges from Ag to U. The optics of the beamline comprises of a double-crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick-Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.

  15. Micro-X-ray fluorescence spectrometer with x-ray single bounce metallic capillary optics for light element analysis (Conference Presentation)

    Science.gov (United States)

    Mroczka, Robert; Żukociński, Grzegorz; Łopucki, Rafał

    2017-05-01

    In the last 20 years, , due to the rapid development of X-ray optics, micro X-ray fluorescence spectrometry (micro-XRF) has become a powerful tool to determine the spatial distribution of major, minor, and trace elements within a sample. Micro-X-ray fluorescence (micro-XRF) spectrometers for light element analysis (6 European Union as part of the Operational Programme Development of Eastern Poland for 2007-2013, Priority I Innovative Economy, Measure I.3. Support for Innovations and The National Centre for Research and Development, Project no. TANGO1,267102/NCBR/2015

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-05-06

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

  17. X-ray fluorescence hologram data collection with a cooled avalanche photodiode

    CERN Document Server

    Hayashi, K; Matsubara, E I; Kishimoto, S; Mori, T; Tanaka, M

    2002-01-01

    A high counting rate X-ray detector with an appropriate energy resolution is desired for high quality X-ray fluorescence hologram measurements because a holographic pattern is detected as extremely small intensity variations of X-ray fluorescence on a large intensity background. A cooled avalanche photodiode (APD), which has about 10% energy resolution and is designed for a high counting rate, fits the above requirements. Reconstructed atomic images from experimental holograms using the APD system provide us a clear view of the first and second neighbor atoms around an emitter. The present result proved that a combination of this APD system and a synchrotron X-ray source enables us to measure a high quality hologram for a reasonable measurement time.

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

    Science.gov (United States)

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

    2014-12-01

    A confocal micro X-ray fluorescence (MXRF) spectrometer based on polycapillary X-ray optics was used for the identification of paint layers. The performance of the confocal MXRF was studied. Multilayered paint fragments of a car were analyzed nondestructively to demonstrate that this confocal MXRF instrument could be used in the discrimination of the various layers in multilayer paint systems. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    OpenAIRE

    Figueroa, Rodolfo; Lozano, Enrique; Valente, Mauro Andres

    2015-01-01

    In-vivo X-ray fluorescence constitutes a useful and accurate technique, worldwide established for constituent elementary distribution assessment. Actually, concentration distributions of arbitrary user-selected elements can be achieved along sample surface with the aim of identifying and simultaneously quantifying every constituent element. The method is based on the use of a collimated X-ray beam reaching the sample. However, one common drawback for considering the application of this techni...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-04-21

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

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

    Science.gov (United States)

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

    2017-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-09-15

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

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

    Science.gov (United States)

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

    2005-01-01

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

  5. High-efficiency logarithmic spiral monochromator for X-ray fluorescence

    CERN Document Server

    Bakulin, A S

    2000-01-01

    A spiral mosaic crystal monochromator system has been designed for high-efficiency collection of X-ray fluorescence. This is especially well suited for X-ray holography measurements, where a weak fluorescence signal must be separated from a strong background. Calculations show that pyrolytic graphite curved to a logarithmic spiral has a dramatically increased angular acceptance compared to standard graphite monochromator designs. The collection efficiency per unit area of graphite is improved by a factor of 200 compared to sagittal focusing geometries, while maintaining the intrinsic graphite energy resolution.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-08-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

  8. Justification and good practice in using handheld portable dental X-ray equipment: a position paper prepared by the European Academy of DentoMaxilloFacial Radiology (EADMFR)

    NARCIS (Netherlands)

    Berkhout, W.E.R.; Suomalainen, A.; Brüllmann, D.; Jacobs, R.; Horner, K.; Stamatakis, H.C.

    2015-01-01

    Handheld portable X-ray devices are increasingly used for intraoral radiography. This development introduces new challenges to staff and patient safety, for which new or revised risk assessments must be made and acted upon prior to use. Major issues might be: difficulties in using rectangular

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

    Science.gov (United States)

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

    Energy Technology Data Exchange (ETDEWEB)

    Sato-Tomita, Ayana, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp; Shibayama, Naoya, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp; Okabe, Takahiro [Division of Biophysics, Department of Physiology, Jichi Medical University, Yakushiji, Shimotsuke 329-0498 (Japan); Happo, Naohisa [Department of Computer and Network Engineering, Graduate School of Information Sciences, Hiroshima City University, Asa-Minami-Ku, Hiroshima 731-3194 (Japan); Kimura, Koji [Department of Physical Science and Engineering, Nagoya Institute of Technology, Gokiso, Showa, Nagoya 466-8555 (Japan); Matsushita, Tomohiro [Japan Synchrotron Radiation Research Institute (JASRI), SPring-8, Sayo, Hyogo 679-5198 (Japan); Park, Sam-Yong [Drug Design Laboratory, Department of Medical Life Science, Yokohama City University, Suehiro, Tsurumi, Yokohama 230-0045 (Japan); Sasaki, Yuji C. [Department of Advanced Material Science, Graduate School of Frontier Science, The University of Tokyo, Kashiwanoha, Kashiwa 277-8561 (Japan); Hayashi, Kouichi, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp [Department of Physical Science and Engineering, Nagoya Institute of Technology, Gokiso, Showa, Nagoya 466-8555 (Japan); Frontier Research Institute for Materials Science, Nagoya Institute of Technology, Gokiso, Showa, Nagoya 466-8555 (Japan)

    2016-06-15

    Experimental procedure and setup for obtaining X-ray fluorescence hologram of crystalline metalloprotein samples are described. Human hemoglobin, an α{sub 2}β{sub 2} 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{sup 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.

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

    Science.gov (United States)

    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.

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

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 25; Issue 5. Development of a total reflection X-ray fluorescence spectrometer for ultra-trace element analysis. M K Tiwari B Gowrishankar V K Raghuvanshi R V Nandedkar K J S Sawhney. Instrumentation Volume 25 Issue 5 October 2002 pp 435-441 ...

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

    2015-02-09

    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 similar to 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.

  14. Chlorophyll fluorescence and X-ray analyses to characterise and improve paddy rice seed quality

    NARCIS (Netherlands)

    Costa, D.S.; Kodde, J.; Groot, S.P.C.

    2014-01-01

    The presence of less-mature seeds or seeds with cracks in a paddy rice seed lot may result in lower seed quality. The potential of chlorophyll fluorescence to provide information on the maturity of single seeds and X-ray analyses to identify seeds with cracks was evaluated in relation to paddy rice

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

    Science.gov (United States)

    Palmer, Peter T.

    2011-01-01

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

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

    DEFF Research Database (Denmark)

    Drabæk, I.; Christensen, Leif Højslet

    1985-01-01

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

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

    DEFF Research Database (Denmark)

    Christensen, Leif Højslet; Pind, Niels

    1982-01-01

    A matrix-independent fundamental parameter-based calibration model for an energy-dispersive X-ray fluorescence spectrometer has been developed. This model, which is part of a fundamental parameter approach quantification method, accounts for both the excitation and detection probability. For each...

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

    Energy Technology Data Exchange (ETDEWEB)

    Kneip, T J; Laurer, G R

    1978-01-01

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

  19. 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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-10-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-12-01

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

  1. Characterization of Roman glass tesserae from the Coriglia excavation site (Italy) via energy-dispersive X-ray fluorescence spectrometry and Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Donais, Mary Kate; Sparks, Andrew; Redente, Monica [Saint Anselm College, Department of Chemistry, Manchester, NH (United States); Pevenage, Jolien van; Moens, Luc; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, Ghent (Belgium); George, David B. [Saint Anselm College, Department of Classics, Manchester, NH (United States); Vandenabeele, Peter [Ghent University, Department of Archaeology, Ghent (Belgium)

    2016-12-15

    The combined use of handheld energy-dispersive X-ray fluorescence spectrometry, Raman spectroscopy, and micro-energy-dispersive X-ray fluorescence spectrometry permitted the characterization of Roman glass tesserae excavation from the Coriglia (Italy) archeological site. Analyses of ten different glass colors were conducted as spot analyses on intact samples and as both spot analyses and line scans on select cross-sectioned samples. The elemental and molecular information gained from these spectral measurements allowed for the qualitative chemical characterization of the bulk glass, decolorants, opacifiers, and coloring agents. The use of an antimony opacifier in many of the samples supports the late Imperial phasing as determined through numismatic, fresco, ceramics, and architectural evidence. And dealinization of the exterior glass layers caused by the burial environment was confirmed. (orig.)

  2. Measurement of mass attenuation coefficients of biological materials by energy dispersive X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ekinci, N. [Science and Art Faculty, Department of Physics, Atatuerk University, 25240 Erzurum (Turkey)]. E-mail: nekinci@atauni.edu.tr; Astam, N. [Faculty of Medicine, Department of Ophthalmology, Atatuerk University, Erzurum (Turkey)

    2007-03-15

    The mass attenuation coefficients for cornea taken from keratitis patient and soft contact lens (-1.75, -3.75, -4 dioptres), leiomyomata uteri and uterus were measured in the X-ray energy (5.9keV) using a SiLi detector and Fe{sup 55} annular source. Full details of the experimental method, experimental set up, the procedure of sample preparation and the results within estimated error are presented. Energy dispersive X-ray fluorescence technique has been successfully used for the determination of the mass attenuation coefficients.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-09-28

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-06-15

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

  5. [Nondestructive imaging of elements distribution in biomedical samples by X-ray fluorescence computed tomography].

    Science.gov (United States)

    Yang, Qun; Deng, Biao; Lü, Wei-Wei; Du, Guo-Hao; Yan, Fu-Hua; Xiao, Ti-Qiao; Xu, Hong-Jie

    2011-10-01

    X-ray fluorescence computed tomography is a stimulated emission tomography that allows nondestructive reconstruction of the elements distribution in the sample, which is important for biomedical investigations. Owing to the high flux density and easy energy tunability of highly collimated synchrotron X-rays, it is possible to apply X-ray fluorescence CT to biomedical samples. Reported in the present paper, an X-ray fluorescence CT system was established at Shanghai Synchrotron Radiation Facility for the investigations of trace elements distribution inside biomedical samples. By optimizing the experiment setup, the spatial resolution was improved and the data acquisition process was obviously speeded up. The maximum-likelihood expectation-maximization algorithm was introduced for the image reconstruction, which remarkably improved the imaging accuracy of element distributions. The developed system was verified by the test sample and medical sample respectively. The results showed that the distribution of interested elements could be imaged correctly, and the spatial resolution of 150 m was achieved. In conclusion, the developed system could be applied to the research on large-size biomedical samples, concerning imaging accuracy, spatial resolution and data collection time.

  6. The application of x-ray fluorescence analysis with total external reflection for determining the microelements in coal

    Energy Technology Data Exchange (ETDEWEB)

    Krasnolutskii, V.P.; Losev, N.F.; Poluyanova, G.I. [Rostov Don State University, Rostov na Donu (Russian Federation)

    1995-09-01

    The results of studying the metrological parameters of a small-size energy dispersive x-ray fluorescence spectrometer with total external reflection of primary radiation are presented. The results of direct x-ray fluorescence measurement of spectral intensities from coal powder sample 1 mg in mass using the spectrometer are in agreement with the data of neutron activation and atomic emission analysis.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-08-01

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

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

    Science.gov (United States)

    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 analysis of low concentrations metals in geological samples and technological products

    Science.gov (United States)

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

    2016-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Spanier, M., E-mail: mspanier@physik.tu-berlin.de; Herzog, C.; Grötzsch, D.; Kramer, F.; Mantouvalou, I.; Malzer, W.; Kanngießer, B. [Institute for Optics and Atomic Physics, Technische Universität Berlin, Hardenbergstraße 36, 10623 Berlin (Germany); Lubeck, J.; Weser, J.; Streeck, C.; Beckhoff, B. [Physikalisch-Technische Bundesanstalt, Abbestraße 2-12, 10587 Berlin (Germany)

    2016-03-15

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-11-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Marques, A.F.; Queralt, I.; Carvalho, M.L. E-mail: luisa@cii.fc.ul.pt; Bordalo, M

    2003-12-15

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-01

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

  15. Use of x-ray fluorescence microprobe and x-ray photoelectron spectroscopy to study variations in bulk and surface chemistry of minerals

    Energy Technology Data Exchange (ETDEWEB)

    Perry, D.L.; Schlueter, E.M. [Lawrence Berkeley National Lab., CA (United States)

    1996-12-31

    Two experimental approaches, synchrotron x-ray fluorescence microprobe and x-ray photoelectron spectroscopy, can be used to study the chemistry of minerals. The former technique yields data at the micron level of depth, whereas the latter approach gives data at the Angstrom level and thus more indicative of the surface conditions of the sample. The present work makes use of the difference in depths being sampled by the two techniques and using them in conjunction with lateral microscopic profiling to study bulk and surface chemistry in oxide and sulfide minerals. A complementary method, angle resolved x-ray photoelectron spectroscopy, is also discussed with respect to both the bulk chemistry and multiple layer films that can occur as reactions products on the surfaces of minerals.

  16. Energy dispersive detector for white beam synchrotron x-ray fluorescence imaging

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, Matthew D., E-mail: Matt.Wilson@stfc.ac.uk; Seller, Paul; Veale, Matthew C. [Science and Technology Facilities Council, Rutherford Appleton Laboratory, Harwell Campus,UK (United Kingdom); Connolley, Thomas [Diamond Light Source, I12 Beamline, Harwell Campus, Didcot, Oxfordshire (United Kingdom); Dolbnya, Igor P.; Malandain, Andrew; Sawhney, Kawal [Diamond Light Source, B16 Beamline, Harwell Campus, Didcot, Oxfordshire (United Kingdom); Grant, Patrick S.; Liotti, Enzo; Lui, Andrew [Department of Materials, University of Oxford Parks Road, Oxford (United Kingdom)

    2016-07-27

    A novel, “single-shot” fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200µm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 µm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 µm pinhole 13 cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm{sup 2} with one of the 80×80 pixels imaging an area equivalent to 13µm{sup 2}. Al-Cu alloys doped with Zr, Ag and Mo were imaged in transmission and fluorescence mode. The fluorescence images showed that the dopant metals could be simultaneously imaged with sufficient counts on all 80x80 pixels within 60 s, with the X-ray flux limiting the fluorescence imaging rate. This technique demonstrated that it is possible to simultaneously image and identify multiple elements on a spatial resolution scale ~10µm or higher without the time consuming need to scan monochromatic energies or raster scan a focused beam of X-rays. Moving to high flux beamlines and using an array of detectors could improve the imaging speed of the technique with element specific imaging estimated to be on a 1 s timescale.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-15

    Superparamagnetic iron oxide (SPIO) nanoparticles are widely used as contrast agents for nuclear magnetic resonance imaging (MRI), and can be modified for improved imaging or to become tissue-specific or even protein-specific. The knowledge of their detailed elemental composition characterisation and potential use in nuclear medicine applications, is, therefore, an important issue. X-ray fluorescence techniques such as particle induced X-ray emission (PIXE) or X-ray fluorescence spectrometry (XRF), can be used for elemental characterisation even in problematic situations where very little sample volume is available. Still, the fluorescence coefficient of Fe is such that, during the decay of the inner-shell ionised atomic structure, keV Auger electrons are produced in excess to X-rays. Since cross-sections for ionisation induced by keV electrons, for low atomic number atoms, are of the order of 10{sup 3} barn, care should be taken to account for possible fluorescence effects caused by Auger electrons, which may lead to the wrong quantification of elements having atomic number lower than the atomic number of Fe. Furthermore, the same electron processes will occur in iron oxide nanoparticles containing {sup 57}Co, which may be used for nuclear medicine therapy purposes. In the present work, simple approximation algorithms are proposed for the quantitative description of radiative and non-radiative processes associated with Auger electrons cascades. The effects on analytical processes and nuclear medicine applications are quantified for the case of iron oxide nanoparticles, by calculating both electron fluorescence emissions and energy deposition on cell tissues where the nanoparticles may be embedded.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-04-01

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

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

    Science.gov (United States)

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

    2015-11-01

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

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

    Science.gov (United States)

    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.

  1. Determination of rare-earth elements in rocks by isotope-excited X-ray fluorescence spectrometry

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar; Wollenberg, H.A.

    1970-01-01

    Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated......-ray spectrometric scan of a longitudinally sliced drill core showed a close correlation between rare-earth abundances and appropriate minerals....

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

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

    Science.gov (United States)

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

    2016-06-01

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

  4. Iodat Analysis Content in Cooking Ingredients Using Iodometry and X-ray Fluorescence Methods.

    OpenAIRE

    Nelson Saksono

    2010-01-01

    Iodat Analysis Content in Cooking Ingredients Using Iodometry and X-ray Fluorescence Methods. Salt iodization program using iodine fortification into salt method is the best method that is effective and economical to overcome the problems caused by iodine deficiency. However in, its development there are some issues clamed that the use of iodized salt is ineffective since iodine content reduces, even disappear when the salt mix with other cooking ingredients. In order to investigated the exis...

  5. Iodat Analysis Content in Cooking Ingredients Using Iodometry and X-ray Fluorescence Methods.

    Directory of Open Access Journals (Sweden)

    Nelson Saksono

    2010-10-01

    Full Text Available Iodat Analysis Content in Cooking Ingredients Using Iodometry and X-ray Fluorescence Methods. Salt iodization program using iodine fortification into salt method is the best method that is effective and economical to overcome the problems caused by iodine deficiency. However in, its development there are some issues clamed that the use of iodized salt is ineffective since iodine content reduces, even disappear when the salt mix with other cooking ingredients. In order to investigated the existence of iodine in cooking ingredients, a research applying iodometry and X-ray fluorescence methods was carry out. The result obtained by iodometry method showed decreases in iodine content in each ingredient, as chili was 75,5 %, ketumbar was 51,43 %, and pepper was 20.99 %. On the other hand, the X-ray Fluorescence measurement showed the iodat deficiency in chili was 12.84 %, ketumbar was 6.42 %, and pepper was 1.14 %. The difference in the result of iodat deficiency can be caused by difference in principle and possessed by them. Iodometry only can analyze iodine in iodat form, while in cooking ingredients iodat may exist in various compound. X-ray Fluorescence can analyze iodat in some compounds so that the complicated matrix ingredient with not interfere the measurement.                                                                          

  6. Analisis Iodat dalam Bumbu Dapur dengan Metode Iodometri dan X-ray Fluorescence

    OpenAIRE

    Nelson Saksono

    2002-01-01

    Iodat Analysis Content in Cooking Ingredients Using Iodometry and X-ray Fluorescence Methods. Salt iodization program using iodine fortification into salt method is the best method that is effective and economical to overcome the problems caused by iodine deficiency. However in, its development there are some issues clamed that the use of iodized salt is ineffective since iodine content reduces, even disappear when the salt mix with other cooking ingredients. In order to investigated the exis...

  7. Measurements of Strontium Levels in Human Bone In Vivo Using Portable X-ray Fluorescence (XRF).

    Science.gov (United States)

    Specht, Aaron J; Mostafaei, Farshad; Lin, Yanfen; Xu, Jian; Nie, Linda H

    2017-08-01

    Measurement of bone strontium (Sr) is vital to determining the effectiveness of Sr supplementation, which is commonly used for the treatment of osteoporosis. Previous technology uses radioisotope sources and bulky equipment to measure bone Sr. This study demonstrates the effectiveness of portable X-ray fluorescence (XRF) for bone Sr measurement and validates it using data from a population of 238 children. We identified correlations between bone Sr and age in our participants.

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

    Science.gov (United States)

    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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Mans, Christian [University of Applied Sciences Muenster, Department of Chemical Engineering, Advanced Analytical Chemistry, Stegerwaldstr. 39, 48565 Steinfurt (Germany)], E-mail: c.mans@fh-muenster.de; Hanning, Stephanie [University of Applied Sciences Muenster, Department of Chemical Engineering, Advanced Analytical Chemistry, Stegerwaldstr. 39, 48565 Steinfurt (Germany)], E-mail: hanning@fh-muenster.de; Simons, Christoph [University of Applied Sciences Muenster, Department of Chemical Engineering, Advanced Analytical Chemistry, Stegerwaldstr. 39, 48565 Steinfurt (Germany)], E-mail: simons@fh-muenster.de; Wegner, Anne [University of Applied Sciences Muenster, Department of Chemical Engineering, Advanced Analytical Chemistry, Stegerwaldstr. 39, 48565 Steinfurt (Germany)], E-mail: awegner@fh-muenster.de; Janssen, Anton [University of Applied Sciences Muenster, Department of Chemical Engineering, Advanced Analytical Chemistry, Stegerwaldstr. 39, 48565 Steinfurt (Germany)], E-mail: janssena@fh-muenster.de; Kreyenschmidt, Martin [University of Applied Sciences Muenster, Department of Chemical Engineering, Advanced Analytical Chemistry, Stegerwaldstr. 39, 48565 Steinfurt (Germany)], E-mail: martin.kreyenschmidt@fh-muenster.de

    2007-02-15

    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.

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

    Science.gov (United States)

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

    2007-02-01

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

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

    Science.gov (United States)

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

    2012-05-15

    Confocal micro-beam X-ray fluorescence microscope was constructed. The system was assembled from commercially available components - a low power X-ray tube source, polycapillary X-ray optics and silicon drift detector - controlled by an in-house developed LabVIEW software. A video camera coupled to optical microscope was utilized to display the area excited by X-ray beam. The camera image calibration and scan area definition software were also based entirely on LabVIEW code. Presently, the main area of application of the newly constructed spectrometer is 2-dimensional mapping of element distribution in environmental, biological and geological samples with micrometer spatial resolution. The hardware and the developed software can already handle volumetric 3-D confocal scans. In this work, a front panel graphical user interface as well as communication protocols between hardware components were described. Two applications of the spectrometer, to homogeneity testing of titanium layers and to imaging of various types of grains in air particulate matter collected on membrane filters, were presented. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  14. Correction of X-ray absorption spectra for thickness inhomogeneity and fluorescence of sample

    CERN Document Server

    Babanov, Y A; Miyanaga, T

    2001-01-01

    For thin powder samples, the EXAFS spectra are often tampered due to the thickness inhomogeneity, and, thick samples, due to the fluorescence at energies above the absorption edge. As a result, the EXAFS amplitude decreases and information about the coordination numbers is distorted. To correct the X-ray absorption spectra for inhomogeneity and fluorescence effects, we propose a new method, which comes to solve the inverse problem. Model calculations were carried out. This method is applied to preliminary processing EXAFS spectra for Ni-Mn alloys.

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

    Energy Technology Data Exchange (ETDEWEB)

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Van Pevenage, Jolien [Ghent University, Department of Analytical Chemistry, Raman Spectroscopy Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); De Langhe, Kaat [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Gent (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Gent (Belgium); Martens, Maximiliaan P.J. [Ghent University, Department of Art, Music and Theatre Sciences, Blandijnberg 2, B-9000 Gent (Belgium)

    2014-07-01

    “Mad Meg”, a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO{sub 2} + 15% K{sub 2}O + 10% CoO + 5% Al{sub 2}O{sub 3}) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel. - Highlights: • In situ, non-destructive investigation of a famous painting by Pieter Bruegel. • Use of a new, commercial available, portable XRF/XRD instrumentation. • Multi-methodological approach: make also use of a mobile Raman spectrometer. • Used pigments and different preparation layers of the painting are characterized. • The verification of two important historical iconographic hypotheses are performed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-08-01

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

  17. PyXRF: Python-based X-ray fluorescence analysis package

    Science.gov (United States)

    Li, Li; Yan, Hanfei; Xu, Wei; Yu, Dantong; Heroux, Annie; Lee, Wah-Keat; Campbell, Stuart I.; Chu, Yong S.

    2017-09-01

    We developed a python-based fluorescence analysis package (PyXRF) at the National Synchrotron Light Source II (NSLS-II) for the X-ray fluorescence-microscopy beamlines, including Hard X-ray Nanoprobe (HXN), and Submicron Resolution X-ray Spectroscopy (SRX). This package contains a high-level fitting engine, a comprehensive commandline/ GUI design, rigorous physics calculations, and a visualization interface. PyXRF offers a method of automatically finding elements, so that users do not need to spend extra time selecting elements manually. Moreover, PyXRF provides a convenient and interactive way of adjusting fitting parameters with physical constraints. This will help us perform quantitative analysis, and find an appropriate initial guess for fitting. Furthermore, we also create an advanced mode for expert users to construct their own fitting strategies with a full control of each fitting parameter. PyXRF runs single-pixel fitting at a fast speed, which opens up the possibilities of viewing the results of fitting in real time during experiments. A convenient I/O interface was designed to obtain data directly from NSLS-II's experimental database. PyXRF is under open-source development and designed to be an integral part of NSLS-II's scientific computation library.

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

    Science.gov (United States)

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

    2014-03-01

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

  19. Sum rule distortions in fluorescence-yield x-ray magnetic circular dichroism

    Science.gov (United States)

    Liu, Boyang; Piamonteze, Cinthia; Delgado-Jaime, Mario Ulises; Wang, Ru-Pan; Heidler, Jakoba; Dreiser, Jan; Chopdekar, Rajesh; Nolting, Frithjof; de Groot, Frank M. F.

    2017-08-01

    The quantitative analysis of 3 d transition metal L2 ,3 edge x-ray magnetic circular dichroism (XMCD) spectra and the related sum rules are compared for measurements with electron yield and fluorescence yield detection. Multiplet calculations on divalent ions show that fluorescence yield detected sum rule derived expectation values of Lz and Sz show noticeable deviations and detection angle dependence. We show that small deviations of the polarization dependent fluorescent decay values lead to significant deviations in the Lz and Sz sum rule values. Fe and Co experimental XMCD spectra of a supported 10 nm CoFe2O4 thin film are measured simultaneously by both electron and fluorescence yield. The deviations shown in the experimental data are well explained by the calculations and are shown to mainly depend on the polarization dependent total decay. We conclude that fluorescence yield detected x-ray magnetic circular dichroism is unsuitable for quantitative analysis of the Lz and Sz sum rule values.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-06

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

  2. A wavelet-based Gaussian method for energy dispersive X-ray fluorescence spectrum

    Directory of Open Access Journals (Sweden)

    Pan Liu

    2017-05-01

    Full Text Available This paper presents a wavelet-based Gaussian method (WGM for the peak intensity estimation of energy dispersive X-ray fluorescence (EDXRF. The relationship between the parameters of Gaussian curve and the wavelet coefficients of Gaussian peak point is firstly established based on the Mexican hat wavelet. It is found that the Gaussian parameters can be accurately calculated by any two wavelet coefficients at the peak point which has to be known. This fact leads to a local Gaussian estimation method for spectral peaks, which estimates the Gaussian parameters based on the detail wavelet coefficients of Gaussian peak point. The proposed method is tested via simulated and measured spectra from an energy X-ray spectrometer, and compared with some existing methods. The results prove that the proposed method can directly estimate the peak intensity of EDXRF free from the background information, and also effectively distinguish overlap peaks in EDXRF spectrum.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  4. Quantitative X-ray fluorescence analysis at the ESRF ID18F microprobe

    CERN Document Server

    Vekemans, B; Somogyi, A; Drakopoulos, M; Kempenaers, L; Simionovici, A; Adams, F

    2003-01-01

    The new ID18F end-station at the European synchrotron radiation facility (ESRF) in Grenoble (France) is dedicated to sensitive and accurate quantitative micro-X-ray fluorescence (XRF) analysis at the ppm level with accuracy better than 10% for elements with atomic numbers above 18. For accurate quantitative analysis, given a high level of instrumental stability, major steps are the extraction and conversion of experimental X-ray line intensities into elemental concentrations. For this purpose a two-step quantification approach was adopted. In the first step, the collected XRF spectra are deconvoluted on the basis of a non-linear least-squares fitting algorithm (AXIL). The extracted characteristic line intensities are then used as input for a detailed Monte Carlo (MC) simulation code dedicated to XRF spectroscopy taking into account specific experimental conditions (excitation/detection) as well as sample characteristics (absorption and enhancement effects, sample topology, heterogeneity etc.). The iterative u...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-09-21

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

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

    Science.gov (United States)

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

    2009-11-15

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

  7. A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

    Science.gov (United States)

    Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

    2017-10-01

    Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

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

    Science.gov (United States)

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

    2008-12-01

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

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

    Science.gov (United States)

    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.

  10. Anomalous scattering, transport, and spatial distribution of X-ray fluorescence at the exit of polycapillary structures

    Energy Technology Data Exchange (ETDEWEB)

    Mazuritskiy, M. I., E-mail: mazurmik@gmail.com; Lerer, A. M.; Makhno, P. V. [Southern Federal University (Russian Federation)

    2016-12-15

    The angular distribution of the X-ray intensity at the exit of microchannel plates at grazing incidence of monochromatic radiation on the walls of microcapillaries has been investigated. The angles and energies of the primary radiation quanta at which the synchrotron beam excites X-ray fluorescence propagating inside polycapillary structures have been determined. The angular dependences of the intensity distribution of X-rays transmitted through the microcapillaries have been studied theoretically and experimentally for energies corresponding to the region of anomalous dispersion near the L{sub 2,3} absorption edges of silicon. The propagation of waves in hollow polycapillary waveguides, the excitation of X-ray fluorescence, and the X-ray diffraction at the exit of microchannel plates have been modeled mathematically. The mathematical model takes into account the presence of a transition layer on the microchannel surface.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

  13. An x-ray fluorescence imaging system for gold nanoparticle detection.

    Science.gov (United States)

    Ricketts, K; Guazzoni, C; Castoldi, A; Gibson, A P; Royle, G J

    2013-11-07

    Gold nanoparticles (GNPs) may be used as a contrast agent to identify tumour location and can be modified to target and image specific tumour biological parameters. There are currently no imaging systems in the literature that have sufficient sensitivity to GNP concentration and distribution measurement at sufficient tissue depth for use in in vivo and in vitro studies. We have demonstrated that high detecting sensitivity of GNPs can be achieved using x-ray fluorescence; furthermore this technique enables greater depth imaging in comparison to optical modalities. Two x-ray fluorescence systems were developed and used to image a range of GNP imaging phantoms. The first system consisted of a 10 mm(2) silicon drift detector coupled to a slightly focusing polycapillary optic which allowed 2D energy resolved imaging in step and scan mode. The system has sensitivity to GNP concentrations as low as 1 ppm. GNP concentrations different by a factor of 5 could be resolved, offering potential to distinguish tumour from non-tumour. The second system was designed to avoid slow step and scan image acquisition; the feasibility of excitation of the whole specimen with a wide beam and detection of the fluorescent x-rays with a pixellated controlled drift energy resolving detector without scanning was investigated. A parallel polycapillary optic coupled to the detector was successfully used to ascertain the position where fluorescence was emitted. The tissue penetration of the technique was demonstrated to be sufficient for near-surface small-animal studies, and for imaging 3D in vitro cellular constructs. Previous work demonstrates strong potential for both imaging systems to form quantitative images of GNP concentration.

  14. Fluorescent intensifying screens: contribution of secondary X-rays; Placas radiograficas amplificadoras: estudo da contribuicao dos raios-X secundarios

    Energy Technology Data Exchange (ETDEWEB)

    Barroso, R.C. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Fisica; Goncalves, O.D. [Universidade do Estado, Rio de Janeiro, RJ (Brazil). Inst. de Fisica; Eichler, J. [Technische Fachhochschule Berlin (Germany). Phys. Technik/Medizinphysik; Lopes, R.T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Lab. de Instrumentacao Nuclear; Cardoso, S.C

    1996-12-31

    The counting rate and angular distribution of secondary X-rays produced by fluorescent intensifying screens are studied. A source of {sup 241} Am - gamma radiation of 59.54 keV - is used. Fluorescent intensifying screens reduce the radiation dose in radiology since they produce visible light which increases the efficiency of the film. In addition, secondary X-rays arise due to the photoelectric effect, elastic (Rayleigh) and inelastic (Compton) scattering 4 refs., 3 figs.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2013-11-01

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

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

    CERN Document Server

    Adams, F

    2003-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-11-15

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

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

    Science.gov (United States)

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

    2016-04-01

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

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

    Science.gov (United States)

    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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-03-10

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

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

    DEFF Research Database (Denmark)

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

    in irradiated U02 fuel samples. About 0.1 mm thin s l i c e s of fuel p e l l e t s (full cross sections) are irradiated by 50 keV X-rays. The i n t e n s i t y of the Xe (Cs, Ba) Ko fluorescence radiation generated i s measured by means of a Ge detector f i t t ed with a collimator. The s l i t i s 0.5 mm wide...

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

    DEFF Research Database (Denmark)

    Schreiber, Norman; Garcia, Emanuel; Kroon, Aart

    2014-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Bauerochse, Andreas

    2013-04-01

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

  7. Application of energy dispersive X-ray fluorescence spectrometry (EDX) in a case of methomyl ingestion.

    Science.gov (United States)

    Kinoshita, Hiroshi; Tanaka, Naoko; Jamal, Mostofa; Kumihashi, Mitsuru; Okuzono, Ryota; Tsutsui, Kunihiko; Ameno, Kiyoshi

    2013-04-10

    We applied energy dispersive X-ray fluorescence spectrometry (EDX) in a case of poisoning by methomyl, a carbamate pesticide. Quantitative GC/MS analysis showed that the concentration of methomyl-oxime in the femoral blood was 4.0 μg/ml. The elemental analysis by EDX identified the high peak of silicon and sulfur in the stomach contents. We concluded that the cause of his death was methomyl poisoning. This indicates that screening of stomach contents by EDX provides useful information for the forensic diagnosis. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  8. X-ray fluorescence holography studies for a Cu{sub 3}Au crystal

    Energy Technology Data Exchange (ETDEWEB)

    Dąbrowski, K.M., E-mail: karol.dabrowski@uj.edu.pl; Dul, D.T.; Jaworska-Gołąb, T.; Rysz, J.; Korecki, P.

    2015-12-01

    In this work we show that performing a numerical correction for beam attenuation and indirect excitation allows one to fully restore element sensitivity in the three-dimensional reconstruction of the atomic structure. This is exemplified by a comparison of atomic images reconstructed from holograms measured for ordered and disordered phases of a Cu{sub 3}Au crystal that clearly show sensitivity to changes in occupancy of the atomic sites. Moreover, the numerical correction, which is based on quantitative methods of X-ray fluorescence spectroscopy, was extended to take into account the influence of a disturbed overlayer in the sample.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

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

    Science.gov (United States)

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

    2014-09-01

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

  11. Multispecies Biofilms Transform Selenium Oxyanions into Elemental Selenium Particles: Studies Using Combined Synchrotron X-ray Fluorescence Imaging and Scanning Transmission X-ray Microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Soo In; George, Graham N.; Lawrence, John R.; Kaminskyj, Susan G. W.; Dynes, James J.; Lai, Barry; Pickering, Ingrid J.

    2016-10-04

    Selenium (Se) is an element of growing environmental concern, because low aqueous concentrations can lead to biomagnification through the aquatic food web. Biofilms, naturally occurring microbial consortia, play numerous important roles in the environment, especially in biogeochemical cycling of toxic elements in aquatic systems. The complexity of naturally forming multispecies biofilms presents challenges for characterization because conventional microscopic techniques require chemical and physical modifications of the sample. Here, multispecies biofilms biotransforming selenium oxyanions were characterized using X-ray fluorescence imaging (XFI) and scanning transmission X-ray microscopy (STXM). These complementary synchrotron techniques required minimal sample preparation and were applied correlatively to the same biofilm areas. Sub-micrometer XFI showed distributions of Se and endogenous metals, while Se K-edge X-ray absorption spectroscopy indicated the presence of elemental Se (Se0). Nanoscale carbon K-edge STXM revealed the distributions of microbial cells, extracellular polymeric substances (EPS), and lipids using the protein, saccharide, and lipid signatures, respectively, together with highly localized Se0 using the Se LIII edge. Transmission electron microscopy showed the electron-dense particle diameter to be 50–700 nm, suggesting Se0 nanoparticles. The intimate association of Se0 particles with protein and polysaccharide biofilm components has implications for the bioavailability of selenium in the environment.

  12. Medieval glass from the Cathedral in Paderborn: a comparative study using X-ray absorption spectroscopy, X-ray fluorescence, and inductively coupled laser ablation mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Hormes, J. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Louisiana State University, CAMD, Baton Rouge, LA (United States); Roy, A.; Bovenkamp, G.L. [Louisiana State University, CAMD, Baton Rouge, LA (United States); Simon, K. [University of Goettingen, Geochemistry, Centre for Geosciences, Goettingen (Germany); Kim, C.Y. [University of Saskatchewan, Canadian Light Source Inc., Saskatoon, SK (Canada); Boerste, N. [Faculty for Theology Paderborn, Paderborn (Germany); Gai, S. [LWL - Archaeologie fuer Westfalen, Muenster (Germany)

    2013-04-15

    We have investigated four stained glass samples recovered from an archaeological excavation at the Cathedral in Paderborn (Germany) between 1978 and 1980. On two of the samples there are parts of paintings. Concentrations of major elements were determined using two independent techniques: LA-ICP-MS (a UV laser ablation microsampler combined with an inductively coupled plasma mass spectrometer) and synchrotron radiation X-ray excited X-ray fluorescence (SR-XRF). The SR-XRF data were quantified by using the program package PyMCA developed by the software group of the ESRF in Grenoble. Significant differences were found between the concentrations determined by the two techniques that can be explained by concentration gradients near the surface of the glasses caused, for example, by corrosion/leaching processes and the different surface sensitivities of the applied techniques. For several of the elements that were detected in the glass and in the colour pigments used for the paintings X-ray absorption near edge structure (XANES) spectra were recorded in order to determine the chemical speciation of the elements of interest. As was expected, most elements in the glass were found as oxides in their most stable form. Two notable exceptions were observed: titanium was not found as rutile - the most stable form of TiO{sub 2} - but in the form of anatase, and lead was not found in one defined chemical state but as a complex mixture of oxide, sulphate, and other compounds. (orig.)

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

    Science.gov (United States)

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

    2016-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-08-31

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-01-01

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

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

    Science.gov (United States)

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

    2014-10-01

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

  17. Quantification of metals in lipstick by energy dispersive X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Wouk, Luana Cristina; Melquiades, Fabio Luiz [Universidade Estadual do Centro Oeste (UNICENTRO), PR (Brazil). Dept. de Fisica

    2011-07-01

    Full text: The objective of this work is to analyze lipstick and lip balm by Energy Dispersive X-Ray Fluorescence and verify if the concentration of the found elements are in accordance with federal rules. Two lip balm and 30 lipstick commercially available were analyzed without preparation. The samples were rubbed on a mylar film until they form a relatively homogeneous layer over entire surface of the film. The superficial density of the samples ranged from 0,0004 to 0,015 g cm{sup -2} , which characterize thin film geometry. Sensitivity values were determined using MicroMatter standards. The measurement system, from Applied Nuclear Physics Laboratory of UEL, consists in a Si-PIN X-ray detector (221 eV resolution for 5,9 keV line, 25 {mu}m Be window) and a mini X-ray tube (4W, Ag target, 50 {mu}m Ag filter). One of the lip balm presented 2620 {+-} 477 {mu}g g{sup -1} of Ti and in the other sample none inorganic elements, which characterize a formulation based on organic compounds. In the lipstick were found the following elements and the number of samples in which it appears, with its respective range of concentration in {mu}g g{sup -1}: Ti (17) 691 to 12721, Fe (22) 237 to 16377, Zn (3) 105 to 2850, Br (2) 510 to 3097, Sr(4) 254 to 1170, Ba (2) 58170 to 90506 and Bi (1) 16275 {+-} 798. According to Brazilian federal rules (ANVISA 79.094) it is not permitted the presence of As and Pb in the formulations. The methodology demonstrated to be suitable for quantification of metals at in natura samples of lipsticks, discarding sample preparation. In sequence a detailed study of the influence of these elements on human health will be performed. (author)

  18. X-ray fluorescence analysis in environmental radiological surveillance using HPGe detectors

    Energy Technology Data Exchange (ETDEWEB)

    Herrera Peraza, E. [Department of Environmental Radiological Surveillance, Centro de Investigacion en Materiales Avanzados (CIMAV), P.O. Box 31109, Miguel de Cervantes no. 120, Complejo Industrial Chihuahua, Chihuahua (Mexico)]. E-mail: eduardo.herrera@cimav.edu.mx; Renteria Villalobos, M. [Department of Environmental Radiological Surveillance, Centro de Investigacion en Materiales Avanzados (CIMAV), P.O. Box 31109, Miguel de Cervantes no. 120, Complejo Industrial Chihuahua, Chihuahua (Mexico); Montero Cabrera, M.E. [Department of Environmental Radiological Surveillance, Centro de Investigacion en Materiales Avanzados (CIMAV), P.O. Box 31109, Miguel de Cervantes no. 120, Complejo Industrial Chihuahua, Chihuahua (Mexico); Munoz Romero, A. [Department of Environmental Radiological Surveillance, Centro de Investigacion en Materiales Avanzados (CIMAV), P.O. Box 31109, Miguel de Cervantes no. 120, Complejo Industrial Chihuahua, Chihuahua (Mexico)

    2004-10-08

    X-ray fluorescence (XRF) has been proven to be a valuable tool for determining trace quantities of heavy metals, such as uranium and lead, in different types of samples. The present paper demonstrates the applicability of XRF spectrometry to measure the concentrations of these heavy metals in samples from natural ore and soil. The values of uranium concentrations in rock from the Pena Blanca uranium ore, in Chihuahua, Mexico, were calculated for the purpose of precertifying the rock powders samples. The comparison with other techniques, such as inductively coupled plasma atomic emission spectrometry, atomic absorption spectrometry, alpha spectrometry and electron microscopy, was used to complete the precertification process, so that the sample powders may be used as secondary standards. The source-sample-detector geometry and the incident angle are the most important factors for obtaining low detection limits. The selected system uses a {sup 57}Co source of about 0.1 mCi to excite the K X-rays from uranium and lead. X-rays were recorded on a CANBERRA HPGe coaxial detector. The comparative results for two incident angles (90 deg and 180 deg ) performed previously by other authors show that the best geometry is the backscattering geometry. In the present paper, using EGS4 code system with Monte Carlo simulation, it was possible to determine the location and distribution of background produced by the Compton edge in the optimized geometry. This procedure allowed to find the minimum detectable concentration of uranium and lead, which was experimentally calculated using standards. The possibility of performing in vivo measurements rapidly and easily, as well as the factors affecting accuracy and the minimum detectable concentration in several samples are also discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lawniczak-Jablonska, K. [Lawrence Berkeley National Lab., CA (United States)]|[Institute of Physics, Warsaw (Poland); Jia, J.J.; Underwood, J.H. [Lawrence Berkeley National Lab., CA (United States)] [and others

    1997-04-01

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

  20. Microbialite Biosignature Analysis by Mesoscale X-ray Fluorescence (μXRF) Mapping

    Science.gov (United States)

    Tice, Michael M.; Quezergue, Kimbra; Pope, Michael C.

    2017-11-01

    As part of its biosignature detection package, the Mars 2020 rover will carry PIXL, the Planetary Instrument for X-ray Lithochemistry, a spatially resolved X-ray fluorescence (μXRF) spectrometer. Understanding the types of biosignatures detectable by μXRF and the rock types μXRF is most effective at analyzing is therefore an important goal in preparation for in situ Mars 2020 science and sample selection. We tested mesoscale chemical mapping for biosignature interpretation in microbialites. In particular, we used μXRF to identify spatial distributions and associations between various elements ("fluorescence microfacies") to infer the physical, biological, and chemical processes that produced the observed compositional distributions. As a test case, elemental distributions from μXRF scans of stromatolites from the Mesoarchean Nsuze Group (2.98 Ga) were analyzed. We included five fluorescence microfacies: laminated dolostone, laminated chert, clotted dolostone and chert, stromatolite clast breccia, and cavity fill. Laminated dolostone was formed primarily by microbial mats that trapped and bound loose sediment and likely precipitated carbonate mud at a shallow depth below the mat surface. Laminated chert was produced by the secondary silicification of microbial mats. Clotted dolostone and chert grew as cauliform, cryptically laminated mounds similar to younger thrombolites and was likely formed by a combination of mat growth and patchy precipitation of early-formed carbonate. Stromatolite clast breccias formed as lag deposits filling erosional scours and interstromatolite spaces. Cavities were filled by microquartz, Mn-rich dolomite, and partially dolomitized calcite. Overall, we concluded that μXRF is effective for inferring genetic processes and identifying biosignatures in compositionally heterogeneous rocks.

  1. X-ray Fluorescence Spectroscopy of Pre-Federal American Currency

    Science.gov (United States)

    Raddell, Mark; Manukyan, Khachatur; Aprahamian, Ani; Wiescher, Michael; Jordan, Louis

    2017-09-01

    X-ray Fluorescence Spectroscopy (XRF) was used to study 17th and 18th century Mexican, Potosí, and Massachusetts silver colonial coins from the University of Notre Dame's Rare Books and Special Collections. Using different configurations and devices, we have learned more about the limitations and optimizations of the method. We have developed a moveable stand that may be used for XRF mapping of coin surfaces. We created standard silver alloy materials for quantification of the elemental composition of the coins. Inductively coupled plasma (ICP) spectroscopy was applied to determine the precise composition of the standards for accurate and non-destructive analyses of the colonial coins. XRF measurements were performed using two different XRF spectrometers, in both air and vacuum conditions, as well as an x-ray beam tube of varying diameters from 2 mm, 1 mm, and 0.03 mm. We quantified both the major elements and the bulk and surface impurities for 90 coins. We are using PCA to look at possible correlations between compositions of coinage from different geographical regions. Preliminary data analyses suggest that Massachusetts coins were minted using silver from Latin American sources. These results are of great interest to historians in tracing the origins of the currency. This work was made possible by the Notre Dame College of Science Summer Undergraduate Research Fellowships (COS-SURF).

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

    Energy Technology Data Exchange (ETDEWEB)

    Rizzutto, Marcia A.; Kajiya, Elizabeth M.; Campos, Pedro H.O.V. de; Almeida, Paula A.D., E-mail: rizzutto@if.usp.br, E-mail: elizabethkajiya@gmail.com [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil)

    2013-07-01

    Since 2003 the analyses of artistic and cultural heritage objects at LAMFI-USP (Laboratorio de Analises de Materiais com Feixes Ionicos), initially restricted to ion beam methods, are growing steadily. Since then, alternative methodologies and procedures have been incorporated to better characterize these objects, which possess distinct physical characteristics and also high cultural and monetary value. The examinations in this kind of objects were expanded to other non-destructive analytical techniques like portable EDXRF (Energy Dispersive X-ray Fluorescence) analysis, X-ray radiography, visible photography, UV (ultraviolet) and IR (infrared) light imaging that are helping to better understand these art objects, particularly paintings. These techniques are helping the analyses of the conservation state of the objects and also revealing characteristics of the painter such as underlying drawings, which help understand the creative process of the artist. These new procedures of analysis are aimed to enable better analytic research in archaeology and artistic and cultural heritage objects and to provide results that subsidize authentic investigations of art objects as well as the origin of archaeological artifacts, while stimulating archeometry and 'arteometry' research in Brazilian Museums. (author)

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

    Science.gov (United States)

    Li, Ruizhe; Li, Liang; Chen, Zhiqiang

    2017-02-07

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

  4. Characterization of aerosol in the atmosphere at Syowa Station by X-ray fluorescence spectrometry (XRF

    Directory of Open Access Journals (Sweden)

    Tomoki Aoyama

    2010-12-01

    Full Text Available The particle size distribution has been continuously measured by optical particle counter at Syowa Station. Physical and chemical properties of particulate matter have been analyzed in the laboratory after arriving in Japan. However, the properties of particles may be changed in this case. In the present work, the atmospheric particulate matter at Syowa Station, Antarctica was characterized by X-ray fluorescence spectroscopy (XRF at Syowa Station. The advantages of this method have non destructive, rapid and simple analysis. The particle samples were collected on a Teflon filter; the obtained particles were measured by XRF (HORIBA, X-ray Analytical Microscope XGT-5000 on site soon for elemental analysis. The obtained results show that collected particles mainly contain sea salt (Na, Mg, Cl, K, Ca and soil (Si, Fe origin components. The particles from sea salt and soil origin increased under blizzard and strong wind condition. Sulfur increased in summer, and decreased in winter while particles from sea salt decreased in summer.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

  6. Study on vinasse dynamics in soil using energy dispersive x-ray fluorescence with radioisotopic excitation

    Energy Technology Data Exchange (ETDEWEB)

    Simabuco, S.M. [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia; Nascimento Filho, V.F. [Sao Paulo Univ., Piracicaba, SP (Brazil). Escola Superior de Agricultura Luiz de Queiroz]|[Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)

    1994-05-01

    The distribution of S, Cl, K and Ca along the profiles of two soils of different texture (Red Yellow Podzolic and Dark Red Latosol) treated with amounts of vinasse equivalent to 4000 m{sup 3}/ha were studied using energy dispersive X-ray fluorescence, observing a significant increase in the contents of these elements. The same effect was observed for Cu, Zn, Rb and Sr contents in soils treated with vinasse as compared to the control. The concentrations of Al, Si, Ti, Mn, Fe and Zr could also be evaluated but no significant variation was observed due to the high soil initial concentrations of these elements as compared to the low concentrations in the vinasse. Annular radioactive sources of Fe-55 and Cd-109 were employed for the excitation of these elements in the soil samples, treated or not with vinasse. For the detection of the characteristic X-rays, a Si(Li) semiconductor detector was used, coupled to a multichannel emulation card inserted in a microcomputer. (author). 8 refs, 6 figs, 4 tabs.

  7. Borehole X-Ray Fluorescence Spectrometer (XRFS): User’s Manual, Software Description, and Performance Report

    Science.gov (United States)

    2007-12-01

    Description ...................................................................................................29 X-ray Tube Control ( XTC ...LABORATORY_________________ TR 0703 29 Software Description X-ray Tube Control ( XTC ) Description This module has two main purposes: to display and

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

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO, and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. (1) In addition to 10 major elements, the method provides a gravimetric loss-on-ignition. Note 1—Much of the text of this test method is derived directly from Major element analysis by wavelength dispersive X-ray fluorescence spectrometry, included in Ref (1). 1.2 Interferences, with analysis by WDXRF, may result from mineralogical or other structural effects, line overlaps, and matrix effects. The structure of the...

  9. Application of x-ray fluorescence analysis to investigation of the composition of gunshot residues

    Science.gov (United States)

    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.

  10. 100-OL-1 Operable Unit Field Portable X-Ray Fluorescence (XRF) Analyzer Pilot Study Plans

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-01

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

  12. Portable X-ray Fluorescence Spectrometry for the analyses of Cultural Heritage

    Science.gov (United States)

    Ridolfi, S.

    2012-07-01

    Field Portable Energy Dispersive X Ray Fluorescence (FP-EDXRF) is particularly useful to analyze works of art, mainly because of his noninvasive and multielemental capability. In many situations FP-EDXRF is the only non invasive technique that can be realistically used to gain some information about the chemical composition of precious and unique objects. Many kind of works, such as paintings, bronzes, precious metals alloys, inks, stones, stamps and more can be studied using a field portable EDXRF system. This manuscript highlights some drawbacks that have to be kept in mind to fulfill a valid measurement such as the need for other backup methods to support portable XRF results or the problem of the non-homogeneity of the sample. This manuscript will also present three examples to demonstrate the usefulness of FP-EDXRF with paintings on canvas, ancient bronzes and sulfur surface analyses.

  13. Reconstruction of confocal micro-X-ray fluorescence spectroscopy depth scans obtained with a laboratory setup.

    Science.gov (United States)

    Mantouvalou, Ioanna; Wolff, Timo; Seim, Christian; Stoytschew, Valentin; Malzer, Wolfgang; Kanngiesser, Birgit

    2014-10-07

    Depth profiling with confocal micro-X-ray fluorescence spectroscopy (confocal micro-XRF) is a nondestructive analytical method for obtaining elemental depth profiles in the micrometer region. Up until now, the quantitative reconstruction of thicknesses and elemental concentration of stratified samples has been only possible with monochromatic, thus, synchrotron radiation. In this work, we present a new calibration and reconstruction procedure, which renders quantification in the laboratory feasible. The proposed model uses the approximation of an effective spot size of the optic in the excitation channel and relies on the calibration of the transmission of this lens beforehand. Calibration issues are discussed and validation measurements on thick multielement reference material and a stratified system are presented.

  14. Portable X-ray fluorescence (pXRF applications in tropical Soil Science

    Directory of Open Access Journals (Sweden)

    Bruno Teixeira Ribeiro

    Full Text Available ABSTRACT The X-ray fluorescence (XRF is an analytical technique for determination of elemental composition of different materials. In soils, the XRF has many pedological, environmental and agronomic applications, mainly after the emergence of portable equipments (pXRF. This technique has been recently adopted and successfully used for soil characterization worldwide, but very rare works have been carried out in soils of developing countries. The soil characterization includes the complete elemental composition determination (nutrients, trace and rare-earth elements and allows estimating some soil physical and chemical properties. In Brazil, this technique is still incipient, mainly the use of pXRF, however, it can greatly contribute to soil characterization in-field or in-lab conditions and also replacing methods of soil analyses considered non-environmentally friendly. This review summarizes the XRF technique including principles and the main applications of pXRF in soils highlighting its potential for tropical Soil Science.

  15. Possible use of pattern recognition for the analysis of Mars rover X-ray fluorescence spectra

    Science.gov (United States)

    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.

  16. Multielement analysis of soils: a proposal involving a portable X-ray fluorescence equipment

    Directory of Open Access Journals (Sweden)

    Juliana Terra

    2014-10-01

    Full Text Available Portable instruments are excellent choices to perform precision agriculture since they allow in situ information about soil composition. In such a way, results are obtained quickly and inputs can be applied promptly, depending on the local soil characteristics. This study aims to develop a method to measure inorganic elements at in natura soils using a portable EDXRF (Energy Dispersive X-ray Fluorescence equipment and multivariate calibration through Partial Least Square Regression (PLS. Seven certified reference standards are used to build the PLS models for Si, K, Ca, Mn and Fe. Two standards are separated for external PLS validation. Finally, the results show that a maximum of 21% is obtained for relative deviation.

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

    Science.gov (United States)

    Pardini, L.; El Hassan, A.; Ferretti, M.; Foresta, A.; Legnaioli, S.; Lorenzetti, G.; Nebbia, E.; Catalli, F.; Harith, M. A.; Diaz Pace, D.; Anabitarte Garcia, F.; Scuotto, M.; Palleschi, V.

    2012-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Tellería Narvaez, C.A.; Fernández Alcázar, S.; Barrientos Zamora, F.G.; Chungara Castro, J.; Luna Lauracia, I.; Mamani Tola, H.; Mita Peralta, E.; Muñoz Gosálvez, A.O. [Centro de Investigaciones y Aplicaciones Nucleares (CIAN-Viacha), Viacha (Bolivia, Plurinational State of); Romero Bolaños, L.E. [Instituto Boliviano de Ciencia y Tecnología Nuclear Av. 6 de Agosto 2905, La Paz (Bolivia, Plurinational State of); Ramírez Ávila, G.M., E-mail: gramirez@ulb.ac.be [Instituto de Investigaciones Físicas, Universidad Mayor de San Andrés, Campus Universitario Cota Cota, Casilla 8635, La Paz (Bolivia, Plurinational State of)

    2014-06-15

    As a first step in the evaluation of nutritional levels in Bolivian children (8–13 years-old), we carried out X-Ray Fluorescence measurements in hair samples of children belonging to different social classes and living either in rural areas or in cities. The aim of this study is to contribute to health policies tending to improve the global health of children and consequently avoid malnutrition. Our method intends to have maximum reliability and at the same time be as simple as possible from an experimental point of view. Additionally, we use this method to determine some other elements such as Fe, Cu, Pb, As and Hg, the latter three considered as contaminants that could be present in children living in areas which neighbor mines and industries. This work will be complemented by some biological and medical tests.

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

    DEFF Research Database (Denmark)

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

    2017-01-01

    Elemental analysis by X-ray fluorescence spectrometry (XRF) of solid samples from a biorefinery process was performed to study the behaviour of mineral elements in a process involving hydrothermal pretreatment of biomass (wheat straw, corn stover, sugarcane bagasse, palm oil empty fruit bunches...... were in general low and they only increased in case of addition during the process. No general tendencies were observed for phosphorus, sulphur, and iron concentrations. A prerequisite for XRF elemental analysis was defining an average chemical formula for the organic matrix of process biomass samples....... Based on ultimate elemental analysis of all biomasses, the formula for biomass was C6H8.4O3.5, which was used for all types of samples (raw biomass, pretreated biomass, and lignin residue) and can be used in future XRF analysis of samples of similar process and biomass feedstock as those used...

  1. Multielement-analysis of city waste incineration ash with total reflection X-ray fluorescence (TXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Gerwinski, W.; Goetz, D.; Koelling, S.; Kunze, J.

    1987-06-01

    The toal reflection X-ray fluorescence technique (TXRF) was used for the routine analysis of city waste incineration ash. Subjects of these analyses were digested ashes (a) and aqueous leaching solutions (b). The accuracy of TXRF was estimated in comparison with atomic absorption spectroscopy (AAS) and atomic emission spectroscopy (ICP-AES) measurements. Satisfactory agreement was found between the results of the different methods for both types of samples. In addition to the direct measurements without prior sample preparation sample type (b) was used to compare three different extraction methods. In each case a dithiocarbamate derivative was used as complexing agent. The separation of the precipitate was performed with a silicagel column, by liquid/liquid extraction and by leaching the sample on a quartz target. Satisfying agreement was found between direct measurements and the different extraction methods.

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

    Science.gov (United States)

    Popescu, Bogdan F. Gh; George, Martin J.; Bergmann, Uwe; Garachtchenko, Alex V.; Kelly, Michael E.; McCrea, Richard P. E.; Lüning, Katharina; Devon, Richard M.; George, Graham N.; Hanson, Akela D.; Harder, Sheri M.; Chapman, L. Dean; Pickering, Ingrid J.; Nichol, Helen

    2009-02-01

    Rapid-scanning x-ray fluorescence (RS-XRF) is a synchrotron technology that maps multiple metals in tissues by employing unique hardware and software to increase scanning speed. RS-XRF was validated by mapping and quantifying iron, zinc and copper in brain slices from Parkinson's disease (PD) and unaffected subjects. Regions and structures in the brain were readily identified by their metal complement and each metal had a unique distribution. Many zinc-rich brain regions were low in iron and vice versa. The location and amount of iron in brain regions known to be affected in PD agreed with analyses using other methods. Sample preparation is simple and standard formalin-fixed autopsy slices are suitable. RS-XRF can simultaneously and non-destructively map and quantify multiple metals and holds great promise to reveal metal pathologies associated with PD and other neurodegenerative diseases as well as diseases of metal metabolism.

  3. Validation of X-ray fluorescence spectrometry for determining osseous or dental origin of unknown material.

    Science.gov (United States)

    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. © 2011 American Academy of Forensic Sciences.

  4. Study of archaeological ceramics by total-reflection X-ray fluorescence spectrometry: Semi-quantitative approach

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Ruiz, R. [Universidad Autonoma de Madrid, Facultad de Ciencias, Servicio Interdepartamental de Investigacion, Modulo C-9, Laboratorio de TXRF, Crta. Colmenar, Km 15, Cantoblanco, E-28049, Madrid (Spain)], E-mail: ramon.fernandez@uam.es; Garcia-Heras, M. [Instituto de Historia-CSIC, C/Serrano, 13. E-28001, Madrid (Spain); CENIM-CSIC, Avda. Gregorio del Amo, 8. E-28040, Madrid (Spain)

    2007-10-15

    Total-reflection X-ray fluorescence spectrometry has been compared with Instrumental Neutron Activation Analysis in order to test its potential application to the study of archaeological ceramics in the archaeometric field. Two direct solid non-chemical sample preparation procedures have been checked: solid sedimentation and solid chemical homogenization. For sedimentation procedure, total-reflection X-ray fluorescence allows the analysis of the elemental composition with respect to the size fraction but not the average evaluation of the composition. For solid chemical homogenization procedure, total-reflection X-ray fluorescence provides precise (from 0.8% to 27% of coefficient of variation) and accurate results (from 91% to 110% of recovery) for 15 elements (Cr, Hf, Ni, Rb, Al, Ba, Ca, K, Mn, Ti, V, Cu, Ga, Y and Fe) with an easy sample preparation process of the solid clay and without previous chemical treatment. The influence of the particle sizes has been checked by total-reflection X-ray fluorescence sample angle scans and anomalous behaviors have been found for three additional detected elements: As, Sr and Zn, which can be attributed to interference effects of the mineral grain sizes of their associated chemical phases in the total-reflection X-ray fluorescence interference region. The solid chemical homogenization procedure produces data useful for archaeological interpretation, which is briefly illustrated by a case-study. Finally, the decantation procedure data can be also useful for size chemical speciation and, consequently, for alternative environmental total-reflection X-ray fluorescence applications.

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

    Science.gov (United States)

    Chtcheprov, Pavel; Inscoe, Christina; Burk, Laurel; Ger, Rachel; Yuan, Hong; Lu, Jianping; Chang, Sha; Zhou, Otto

    2014-03-01

    Microbeam radiation therapy (MRT) uses an array of high-dose, narrow (~100 μm) beams separated by a fraction of a millimeter to treat various radio-resistant, deep-seated tumors. MRT has been shown to spare normal tissue up to 1000 Gy of entrance dose while still being highly tumoricidal. Current methods of tumor localization for our MRT treatments require MRI and X-ray imaging with subject motion and image registration that contribute to the measurement error. The purpose of this study is to develop a novel form of imaging to quickly and accurately assist in high resolution target positioning for MRT treatments using X-ray fluorescence (XRF). The key to this method is using the microbeam to both treat and image. High Z contrast media is injected into the phantom or blood pool of the subject prior to imaging. Using a collimated spectrum analyzer, the region of interest is scanned through the MRT beam and the fluorescence signal is recorded for each slice. The signal can be processed to show vascular differences in the tissue and isolate tumor regions. Using the radiation therapy source as the imaging source, repositioning and registration errors are eliminated. A phantom study showed that a spatial resolution of a fraction of microbeam width can be achieved by precision translation of the mouse stage. Preliminary results from an animal study showed accurate iodine profusion, confirmed by CT. The proposed image guidance method, using XRF to locate and ablate tumors, can be used as a fast and accurate MRT treatment planning system.

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

    Energy Technology Data Exchange (ETDEWEB)

    Wolff, Timo

    2009-07-15

    X-ray fluorescence analysis (XRF) is a standard method for non-destructive investigations. Due to the development of polycapillary optics and SDDdetectors requiring no cooling with liquid nitrogen, XRF becomes a suitable method for a large number of applications, e. g. for the analysis of objects in arts and archaeology. Spectrometers developed for those purposes allow investigations outside of laboratories und provide excitation areas with diameters of 10-70 {mu}m. In most applications, quantification of XRF data is realized by the usage of standard reference materials. Due to absorption processes in the samples the accuracy of the results depends strongly on the similarity of the sample and the reference standard. In cases where no suitable references are available, quantification can be done based on the ''fundamental parameter (fp) method''. This quantification procedure is based on a set of equations describing the fluorescence production and detection mathematical. The cross sections for the interaction of x-rays with matter can be taken from different databases. During an iteration process the element concentrations can be determined. Quantitative XRF based on fundamental parameters requires an accurate knowledge of the excitation spectrum. In case of a conventional setup this spectrum is given by the X-ray tube spectrum and can be calculated. The use of polycapillary optics in micro-XRF spectrometers changes the spectral distribution of the excitation radiation. For this reason it is necessary to access the transmission function of the used optic. The aim of this work is to find a procedure to describe this function for routine quantification based on fundamental parameters. Most of the measurements have been carried out using a commercial spectrometer developed for applications in arts and archaeology. On the one hand the parameters of the lens, used in the spectrometer, have been investigated by different experimental characterization

  7. 2D/3D cryo x-ray fluorescence imaging at the bionanoprobe at the advanced photon source

    Energy Technology Data Exchange (ETDEWEB)

    Chen, S., E-mail: sichen@aps.anl.gov; Vine, D. J.; Lai, B. [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Paunesku, T.; Yuan, Y.; Woloschak, G. E. [Department of Radiation Oncology, Northwester University, Chicago, IL 60611 (United States); Deng, J. [Applied Physics, Northwestern University, Evanston, IL 60208 (United States); Jin, Q.; Hong, Y. P. [Department of Physics and Astronomy, Northwestern University, Evanston, IL 60208 (United States); Flachenecker, C.; Hornberger, B. [Carl Zeiss X-ray Microscopy, Pleasanton, CA 94588 (United States); Brister, K. [Synchrotron Research Center, Northwestern University, Argonne, IL 60439 (United States); Jacobsen, C. [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Applied Physics, Northwestern University, Evanston, IL 60208 (United States); Department of Physics and Astronomy, Northwestern University, Evanston, IL 60208 (United States); Chemistry of Life Processes Institute, Northwestern University, Evanston, IL 60208 (United States); Vogt, S. [Advanced Photon Source, Argonne National Laboratory, Lemont, IL 60439 (United States); Department of Radiation Oncology, Northwester University, Chicago, IL 60611 (United States)

    2016-01-28

    Trace elements, particularly metals, play very important roles in biological systems. Synchrotron-based hard X-ray fluorescence microscopy offers the most suitable capabilities to quantitatively study trace metals in thick biological samples, such as whole cells and tissues. In this manuscript, we have demonstrated X-ray fluorescence imaging of frozen-hydrated whole cells using the recent developed Bionanoprobe (BNP). The BNP provides spatial resolution down to 30 nm and cryogenic capabilities. Frozen-hydrated biological cells have been directly examined on a sub-cellular level at liquid nitrogen temperatures with minimal sample preparation.

  8. The Bionanoprobe: Synchrotron-Based Hard X-ray Fluorescence Microscopy for 2D/3D Trace Element Mapping

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Si; Paunesku, Tatjana; Yuan, Ye; Jin, Qiaoling; Finney, Lydia; Hornberger, Benjamin; Flachenecker, Claus; Lai, Barry; Brister, Keith; Jacobsen, Chris; Woloschak, Gayle; Vogt, Stefan

    2015-04-29

    Trace elements, particularly metals, play an important role in a large variety of cellular processes in a biological system. In the context of biological organisms and tissues, the term trace element means that over the entire organisms an element is present at only trace levels, 100ppm or lower. Trace element distribution and content can be analyzed using several techniques, for example, visible light optical fluorescence imaging, energy-dispersive X-ray spectroscopy on an election microscope, synchrotron-based X-ray fluorescence (XRF) imagine,

  9. Synchrotron X-ray fluorescence studies of a bromine-labelled cyclic RGD peptide interacting with individual tumor cells

    Energy Technology Data Exchange (ETDEWEB)

    Sheridan, Erin J.; Austin, Christopher J. D. [School of Chemistry, The University of Sydney, Sydney, NSW 2006 (Australia); Aitken, Jade B. [School of Chemistry, The University of Sydney, Sydney, NSW 2006 (Australia); Australian Synchrotron, Clayton, Victoria 3168 (Australia); Institute of Materials Structure Science, KEK, Tsukuba, Ibaraki 305-0801 (Japan); Vogt, Stefan [X-ray Science Division, Argonne National Laboratory, Argonne, IL 60439 (United States); Jolliffe, Katrina A. [School of Chemistry, The University of Sydney, Sydney, NSW 2006 (Australia); Harris, Hugh H. [School of Chemistry and Physics, The University of Adelaide, Adelaide, South Australia 5005 (Australia); Rendina, Louis M., E-mail: lou.rendina@sydney.edu.au [School of Chemistry, The University of Sydney, Sydney, NSW 2006 (Australia)

    2013-03-01

    The first example of synchrotron X-ray fluorescence imaging of cultured mammalian cells in cyclic peptide research is reported. The study reports the first quantitative analysis of the incorporation of a bromine-labelled cyclic RGD peptide and its effects on the biodistribution of endogenous elements (for example, K and Cl) within individual tumor cells. The first example of synchrotron X-ray fluorescence imaging of cultured mammalian cells in cyclic peptide research is reported. The study reports the first quantitative analysis of the incorporation of a bromine-labelled cyclic RGD peptide and its effects on the biodistribution of endogenous elements (for example, K and Cl) within individual tumor cells.

  10. [Analysis and characterization of Belamcanda chinensis with space mutagenesis breeding by X-ray fluorescence analysis and X-ray diffraction].

    Science.gov (United States)

    Guan, Ying; Ding, Xi-Feng; Wang, Wen-Jing; Guo, Xi-Hua; Zhu, Yan-Ying

    2008-02-01

    The contents of various elements in the fourth generation Belamcanda chinensis (L.) DC. with space mutagenesis breeding were analyzed and characterized. X-ray fluorescence spectrum analysis (XRF) and powder X-ray diffraction (PXRD) were applied jointly. It was found that the content of K element in the space flight mutagenesis increases 1.03 and 0.31 times, Mg enhances 1.44 and 0.06 times, but Al reduces 38.5% and 85.5% respectively compared to the contents in the ground group and the comparison group, while those of Ca, Mn and Fe enhance 0.95, 0.30 and 0.29 times respectively contrasted to the ground group. Besides, there was discovered the crystal of whewellite in the Belamcanda chinensis (L.) DC. and the content in the ground group is less than that of the outer space and the outer space group, which in turn is less than that of the comparison group. It is concluded that the contents of mineral elements indispensable to body in the space group are closer or superior to the comparison, group as compared to the ground group. In the present paper, a quick and simple appraising method is offered, which may be of great significance to the popularization of the planting outer space Chinese traditional medicine to filtrate more excellent breed and set up norm of quality appraisal.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-01-01

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

  12. The aquatic hyphomycete Heliscus lugdunensis protects its hyphae tip cells from cadmium: A micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy study

    Science.gov (United States)

    Isaure, Marie-Pierre; Leyh, Benjamin; Salomé, Murielle; Krauss, Gerd-Joachim; Schaumlöffel, Dirk; Dobritzsch, Dirk

    2017-11-01

    Aquatic fungi can be used to evaluate the functioning of natural ecosystems. Heliscus lugdunensis is an early colonizer of allochthone leafs. Since this aquatic hyphomycete is able to develop in metal contaminated habitats and tolerates cadmium, it appears to be a good candidate to investigate adaptation to metal pollution. This study aimed at examining the sequestration of Cd in the hyphae of H. lugdunensis, and particularly the role of the tip cells. For that, H. lugdunensis growth was evaluated under various Cd concentrations, and a combination of synchrotron micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy was carried out to determine the compartments of Cd accumulation and the Cd chemical species, respectively. Results showed that the hyphal tip cells were depleted in Cd, and that the metal was stored in older cells. Cd was mainly associated with sulfur ligands and to a lesser extent bound to phosphates and carboxyl/hydroxyl groups from cell wall and/or organic acids. Finally, the aquatic fungus was able to maintain the tip cell as a functional system, thus allowing the colonization of contaminated environments.

  13. Investigation of high-resolution superconducting tunnel junction detectors for low-energy X-ray fluorescence analysis

    CERN Document Server

    Beckhoff, B; Ulm, G

    2003-01-01

    The energy resolution of conventional semiconductor detectors is insufficient for simultaneously separating the leading fluorescence lines of low Z and medium Z materials in the soft X-ray regime. It is therefore important to investigate alternative detection instruments offering higher energy resolution and evaluate their applicability to soft X-ray fluorescence (XRF) analysis. In this paper, various results of the characterization and evaluation of a cryogenic superconducting tunnel junction (STJ) detector, which was provided to the Physikalisch-Technische Bundesanstalt (PTB) by the Lawrence Livermore National Laboratory, are given with respect to both detector response functions and XRF. For this investigation, monochromatized undulator radiation of high spectral purity, available to the PTB X-ray radiometry laboratory at the electron storage ring BESSY II, was employed, by which it was possible to record the STJ response functions at various photon energies of interest ranging from 180 to 1600 eV. By scan...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-11-15

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

  16. Ultraviolet germicidal irradiation and its effects on elemental distributions in mouse embryonic fibroblast cells in x-ray fluorescence microanalysis.

    Directory of Open Access Journals (Sweden)

    Qiaoling Jin

    Full Text Available Rapidly-frozen hydrated (cryopreserved specimens combined with cryo-scanning x-ray fluorescence microscopy provide an ideal approach for investigating elemental distributions in biological cells and tissues. However, because cryopreservation does not deactivate potentially infectious agents associated with Risk Group 2 biological materials, one must be concerned with contamination of expensive and complicated cryogenic x-ray microscopes when working with such materials. We employed ultraviolet germicidal irradiation to decontaminate previously cryopreserved cells under liquid nitrogen, and then investigated its effects on elemental distributions under both frozen hydrated and freeze dried states with x-ray fluorescence microscopy. We show that the contents and distributions of most biologically important elements remain nearly unchanged when compared with non-ultraviolet-irradiated counterparts, even after multiple cycles of ultraviolet germicidal irradiation and cryogenic x-ray imaging. This provides a potential pathway for rendering Risk Group 2 biological materials safe for handling in multiuser cryogenic x-ray microscopes without affecting the fidelity of the results.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-11-15

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

  18. Identification of inorganic pigments used in porcelain cards based on fusing Raman and X-ray fluorescence (XRF) data.

    NARCIS (Netherlands)

    Deneckere, A.; de Vries, L.; Vekemans, M.; van de Voorde, L.; Ariese, F.; Vincze, L.; Moens, L.; Vandenabeele, P.

    2011-01-01

    Raman spectroscopy and X-ray fluorescence (XRF) spectroscopy are often used as complementary techniques that are well suited for the analysis of art objects because both techniques are fast, sensitive, and noninvasive and measurements can take place in situ. In most of these studies, both techniques

  19. A Review of Energy Dispersive X-Ray Fluorescence (EDXRF) as an Analytical Tool in Numismatic Studies.

    Science.gov (United States)

    Navas, María José; Asuero, Agustín García; Jiménez, Ana María

    2016-01-01

    Energy dispersive X-ray fluorescence spectrometry (EDXRF) as an analytical technique in studies of ancient coins is summarized and reviewed. Specific EDXRF applications in historical studies, in studies of the corrosion of coins, and in studies of the optimal working conditions of some laser-based treatment for the cleaning of coins are described. © The Author(s) 2015.

  20. Determination of diffusion profiles of silver ions in soda-lime-silica glass by X-ray fluorescence spectrometry

    NARCIS (Netherlands)

    Bos, M.; Boukamp, Bernard A.; Vrielink, J.A.M.

    2002-01-01

    A nondestructive method based on X-ray fluorescence (XRF) spectrometry is presented for the determination of concentration-depth profiles in the top layer of flat solid samples. The method was tested in the determination of the interdiffusion coefficient of silver and sodium ions in soda-lime–silica

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

    NARCIS (Netherlands)

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

    2015-01-01

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

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

    Science.gov (United States)

    Specht, Aaron James

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

  3. Gemas: issues from the comparison of aqua regia and X-ray fluorescence results

    Science.gov (United States)

    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 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 that almost for all

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-04-01

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

  5. The use of various X-ray fluorescence analysis modalities for the investigation of historical paintings: The case study on the Late Gothic panel painting

    Science.gov (United States)

    Bártová, H.; Trojek, T.; Čechák, T.; Šefců, R.; Chlumská, Š.

    2017-10-01

    The presence of heavy chemical elements in old pigments is possible to identify in historical paintings using X-ray fluorescence analysis (XRF). This is a non-destructive analytical method frequently used in examination of objects that require in situ analysis, where it is necessary to avoid damaging the object by taking samples. Different modalities are available, such as microanalysis, scanning selected areas, or depth profiling techniques. Surface scanning is particularly profitable since 2D element distribution maps are much more understandable than the results of individual analyses. Information on the layered structure of the painting can be also obtained by handheld portable systems. Results presented in our paper combine 2D element distribution maps obtained by scanning analysis, and depth profiling using conventional XRF. The latter is very suitable for objects of art, as it can be evaluated from data measured with portable XRF device. Depth profiling by conventional XRF is based on the differences in X-ray absorption in paint layers. The XRF technique was applied for analysis of panel paintings of the Master of the St George Altarpiece who was active in Prague in the 1470s and 1480s. The results were evaluated by taking micro-samples and performing a material analysis.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-10-15

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

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

    Indian Academy of Sciences (India)

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

  8. Local structure analysis of Cu(In,Ga)Se{sub 2} by X-ray fluorescence holography

    Energy Technology Data Exchange (ETDEWEB)

    Shirakata, Sho; Kitamura, Yuma [Faculty of Engineering, Ehime University, Matsuyama 790-8577 (Japan); Happo, Naohisa [Graduate School of Information Sciences, Hiroshima City University, Hiroshima 731-3194 (Japan); Hosokawa, Shinya [Department of Physics, Kumamoto University, Kumamoto 860-8555 (Japan); Hayashi, Kouichi [Faculty of Engineering, Nagoya Institute of technology, Gokiso-cho, Showa-ku, Nagoya, Aichi 466-8555 (Japan)

    2017-06-15

    X-ray Fluorescence Holography (XFH) study of Cu(In,Ga)Se{sub 2} single crystals has been performed using an inverse mode. Energies of incident X-ray are from 9.2 to 13.2 keV. The Cu-Kα X-ray fluorescence hologram has been constructed, and atomic images were reconstructed using Barton's algorithm. Dependence of fluorescent X-ray, either Cu or Ga, on the reconstructed atomic images of CuIn{sub 0.2}Ga{sub 0.8}Se{sub 2} was examined. The atomic image of CuIn{sub 0.2}Ga{sub 0.8}Se{sub 2} was compared with that of CuIn{sub 0.8}Ga{sub 0.2}Se{sub 2}. The reconstructed atomic images of the cation (Cu, Ga, and In) plane and that of the anion (Se) plane are discussed in terms of the alloy composition. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-15

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-08-01

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

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

    Science.gov (United States)

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

    2017-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Bilo, Fabjola [INSTM and Chemistry for Technologies Laboratory, University of Brescia, via Branze, 38, 25123 Brescia (Italy); Borgese, Laura, E-mail: laura.borgese@unibs.itl [INSTM and Chemistry for Technologies Laboratory, University of Brescia, via Branze, 38, 25123 Brescia (Italy); Prost, Josef; Rauwolf, Mirjam; Turyanskaya, Anna; Wobrauschek, Peter; Kregsamer, Peter; Streli, Christina [Atominstitut, TU Wien, Stadionallee 2, 1020 Vienna (Austria); Pazzaglia, Ugo [Dipartimento Specialità Medico Chirurgiche Sc. Radiol. e Sanità Pubblica, University of Brescia, v.le Europa, 11, 25121 Brescia (Italy); Depero, Laura E. [INSTM and Chemistry for Technologies Laboratory, University of Brescia, via Branze, 38, 25123 Brescia (Italy)

    2015-12-30

    Highlights: • Co and Cr migrate from bare alloy implant to the surrounding tissue showing a cluster distribution. • Co and Cr migrate from the TiO{sub 2} coated implant to the surrounding tissue showing a decreasing gradient distribution from the alloy surface. • TiO{sub 2} coating layers obtained by ALD on Co–Cr alloy show a barrier effect for the migration of metals. • The thicker the TiO{sub 2} layer deposited by ALD, the lower the metal migration. • The migration of metals from bare alloy toward the surrounding tissue increases with time. This effect is not detected in the coated samples. - Abstract: 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 TiO{sub 2}. 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 TiO{sub 2} layer, the lower is the metal migration.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-08-15

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

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

    Science.gov (United States)

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

    2010-06-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-08-15

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

  20. Semi-Quantitative Evaluation of Secondary Carbonates via Portable X-ray Fluorescence Spectrometry

    Science.gov (United States)

    Chakraborty, Somsubhra; Weindorf, David; Weindorf, Camille; Duda, Bogdan; Pennington, Sarah; Ortiz, Rebekah

    2017-04-01

    Secondary calcium carbonate commonly occurs in subsoils of semi-arid soils worldwide. In US Soil Taxonomy, such horizons are frequently described as Bk, Bkk, Bkm, Bkkm, or Ck horizons at variable stages of development. Specifically, the Soil Survey Staff uses a qualitative scale of one through six to indicate differential developmental stages. However, considerable disagreement exists even among experienced soil scientists. Evaluating 75 soil samples from across four US states, a portable X-ray fluorescence (PXRF) spectrometer was used to quantify the total soil Ca content and compare it to average developmental stage scores as determined by a panel of Soil Survey Staff personnel. Samples were evaluated both as intact aggregates as well as ground (readings of total soil Ca concentration steadily increased under both conditions as developmental stage progressed. However, minimal difference was observed between stage five and six carbonate accumulation. Stage three showed the widest variability in total soil Ca. Given than PXRF cannot distinguish between primary and secondary CaCO3 in soils, interpretation by the analyst remains essential. Nonetheless, PXRF provides an important tool for assessing carbonate laden subsoils providing elemental differentiation beyond that perceived by the human eye.

  1. Downsizing of Johansson spectrometer for X-ray fluorescence trace analysis with brilliant undulator source

    CERN Document Server

    Sakurai, K; Inoue, K; Yagi, N

    2001-01-01

    The downsizing of a Johansson-type X-ray fluorescence (XRF) spectrometer has been examined as a way of enhancing detection efficiency with a tolerable loss of energy resolution. A compact spectrometer equipped with a Ge(2 2 0) analyzing crystal with a Rowland radius of 120 mm has been tested with a highly brilliant helical undulator source at BL40XU, SPring-8. The energy resolution obtained for cobalt K alpha sub 1 (6930.32 eV) was 8.8 eV, which is 10-20 times better than that obtained using a Si(Li) detector, and effectively improved the signal-to-background ratio for XRF spectra. The combination of the present spectrometer and a third generation synchrotron source could provide new opportunities for trace analytical applications, which have been difficult so far by conventional synchrotron XRF experiments based on a Si(Li) detector system. The detection limit obtained for solid bulk samples has reached a level of several tens of ppb.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-01

    Hydrogen Peroxide's a bleaching agent capable of oxidizing a wide range of colored organic, causing discoloration and hence bleaching of the substrate, but some authors related the occurrence of side effects related to bleaching of the tooth structure, such as changes in morphology superficial. It was used 6 bovine incisors, each tooth was initially evaluated six times in different areas to obtain the count of elements phosphorus and calcium using X-Ray Fluorescence. The teeth were randomly divided in two groups: both groups were submitted to bleaching in office with hydrogen peroxide 38%, once a week during three weeks. Group 1 was stored in distilled water and group 2 in artificial saliva, between the sessions. The measurements were repeated every seven days before the bleaching treatment. Besides that, changes in mineral levels were always assessed in the same area and using the same procedure. It was observed that the bleaching was not able to demineralize the tooth enamel studied. (author)

  3. Archaeology of Chilean pre-hispanic pieces using induced x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Morales, J.R.; Dinator, M.I. [Universidad de Chile, Facultad de Ciencias, Santiago (Chile); Tellez, F. [Universidad Catolica del Norte, I.I.A. San Pedro de Atacama (Chile)

    2001-09-01

    Full text: One of the most famous archaeological sites of Chile is San Pedro de Atacama in the north Andean highlands. The site, 68.23 W, 22.89 S, is close to the border lines with Argentina and Bolivia and was occupied by different cultures in the past like Atacameos and lately by Incas in s. X V. About a century later Hispanic explorers visited the zone. The area is rich in tombs and remains. Due to the abundance of minerals, metallurgy was practiced by pre-Hispanic cultures. This work is part of a study concerning the characterization of metallic artifacts found in several excavations. The elemental composition can help in determining the provenance of the pieces, and the metallurgical techniques used. A set of twenty pieces including hatchets, knifes, chisels, maces and bells were analyzed by X ray fluorescence induced by photons of 59.5 keV provided by a source of Am-241. Detection of Mn, Fe, Ni, Cu, As, Zr, Ag, Sn, Sb, Ba, and Pb has allowed determination of their provenance. (Author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Pepponi, G. E-mail: pepponi@itc.it; Lazzeri, P.; Coghe, N.; Bersani, M.; Gottardini, E.; Cristofolini, F.; Clauser, G.; Torboli, A

    2004-08-31

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

  5. X-ray fluorescence spectrometry using Synchrotron Radiation with applications in unmanned aircraft environmental sensing

    Science.gov (United States)

    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

  6. Lead tolerance and cellular distribution in Elsholtzia splendens using synchrotron radiation micro-X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jie [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China); Tian, Shengke [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China); University of Florida, Institute of Food and Agricultural Science, Indian River Research and Education Center, Fort Pierce, FL 34945 (United States); Lu, Lingli; Shohag, M.J.I.; Liao, Haibing [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China); Yang, Xiaoe, E-mail: xyang@zju.edu.cn [MOE Key Laboratory of Environment Remediation and Ecosystem Health, College of Environmental and Resource Sciences, Zhejiang University, Hangzhou 310058 (China)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer Elsholtzia splendens had a good ability of lead tolerance and accumulation. Black-Right-Pointing-Pointer Pb was mostly restricted to the vascular bundles and epidermis tissues. Black-Right-Pointing-Pointer Pb and Ca shared most similar distribution patterns in E. splendens. - Abstract: Hydroponic experiments were conducted to investigate the tolerance and spatial distribution of lead (Pb) in Elsholtzia splendens-a copper (Cu) accumulator plant using synchrotron-based micro-X-ray fluorescence. According to chlorophyll concentration and chlorophyll fluorescence parameters, E. splendens displayed certain tolerance at 100 {mu}M Pb treatment. Lead concentration in roots, stems and leaves of E. splendens reached 45,183.6, 1657.6, and 380.9 mg kg{sup -1}, respectively. Pb was mostly accumulated in the roots, and there were also high concentrations of Pb been transported into stems and leaves. Micro-XRF analysis of the stem and leaf cross section revealed that Pb was mostly restricted in the vascular bundles and epidermis tissues of both stem and leaf of E. splendens. The correlation between distribution of K, Ca, Zn and Pb were analyzed. There were significant positive correlations (P < 0.01) among Pb and Ca, K, Zn distribution both in stem and leaf of E. splendens. However, among the three elements, Ca shared the most similar distribution pattern and the highest correlation coefficients with Pb in both stem and leaf cross section of E. splendens. This suggests that Ca may play an important role in Pb accumulation in stem and leaf of E. splendens.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Koichiro Hayashi

    2014-12-01

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

  9. Development of a portable system of grazing exit X-Ray fluorescence applied to environmental and biological studies

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Ramon S.; Oliveira, Davi F.; Anjos, Marcelino J. [Universidade do Estado do Rio de Janeiro (UERJ), RJ (Brazil). Instituto de Fisica; Assis, Joaquim T., E-mail: ramonziosp@yahoo.com.br, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br, E-mail: joaquim.iprj@gmail.com [Universidade do Estado do Rio de Janeiro (UERJ), Nova Friburgo, RJ (Brazil). Instituto Politécnico

    2017-07-01

    In this study was developed a portable system of grazing exit X-ray fluorescence (geometric 90° - 0°) that will be applied in environmental studies (aerosol samples) and biological studies. GE-XRF portable system is formed by a mini X-ray tube of low power (anode of Au, maximum voltage and current of 50 kV and 200 μA, respectively) and a SiPIN detector (model XR-100CR of the Amptek). The reflectors used as sample support (sampler carrier) were quartz discs with 25.4 mm diameter and 3.0 mm thickness. The grazing exit angle was experimentally determined by measuring a cooper solution (10 μg.g{sup -1}). The system of GE-XRF proved to be quite stable and reproducible. It was calculated the sensibility curve of the system using multielement solutions. The accuracy of the system was checked using multielement reference solution as standard reference material. The relative errors between measured and certified values are in the range of 4 to 19%. The first results showed a background was drastically reduced at grazing exit angles, enabling trace elemental analysis. This paper shows that it is possible to produce a portable system of grazing exit X-ray fluorescence compact, efficient, low-cost and easy-to-handle instrumentation using a low-power X-ray tube and a SiPIN compact detector. (author)

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

    Indian Academy of Sciences (India)

    Unknown

    TXRF) spectrometer has been designed, constructed and realized. The spectrometer is capable of ultra-trace multielement analysis as well as performs surface characterization of thin films. The TXRF setup comprises of an X-ray generator, a slit-.

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

    Science.gov (United States)

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

    2008-09-01

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

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

    Science.gov (United States)

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

    2015-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-09-21

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

  14. Elemental contents in exotic Brazilian tropical fruits evaluated by energy dispersive X-ray fluorescence

    Directory of Open Access Journals (Sweden)

    Oliveira Alessandra Lopes de

    2006-01-01

    Full Text Available The exotic flavor of Brazilian tropical fruits led to increased consumption. Consumers awareness regarding balanced diets, makes necessary determining nutritional composition - vitamins and minerals of the fruits ordinarily consumed. This study contributed to the evaluation of macro (K, Ca and microelements (Mn, Fe, Cu, Zn and Br in eight exotic Brazilian tropical fruits: "abiu" (Lucuma caimito Ruiz & Pav., "jenipapo" (Genipa americana L., "jambo rosa" (rose apple, Eugenia Jambos L., "jambo vermelho" (Syzygium malaccence L., Merr & Perry, "macaúba" (Acrocomia aculeata Jacq. Lood. Ex Mart., "mangaba" (Hancornia speciosa, "pitanga" (Brazilian Cherry, Eugenia uniflora L., and tamarind (Tamarindus indica L., using the Energy Dispersive X-Ray Fluorescence (EDXRF technique. "jambo vermelho" and "macaúba" presented the highest values of K concentrations, 1,558 and 1,725 mg 100 g-1, respectively. On the other hand, Ca concentrations were highest in "macaúba" (680 mg 100 g-1 and "jenipapo" (341 mg 100 g-1. The microelemental concentrations in these eight fruits ranged from: 0.9 to 2.0 mg 100 g-1 for Mn, 3.9 to 11.4 mg 100 g-1 for Fe, 0.5 to 1.0 mg 100 g-1 for Cu, 0.6 to 1.5 mg 100 g-1 for, Zn and 0.3 to 1.3 mg 100 g-1 for Br. The amounts of macro and microelements in the eight fruits analyzed were compared to other tropical fruits and it was found that some of them could be classified as rich sources for these macro and microelements.

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

    Directory of Open Access Journals (Sweden)

    Monica Baldassarri

    2014-01-01

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

  16. Quantitative analysis of concrete using portable x-ray fluorescence: Method development and validation

    Energy Technology Data Exchange (ETDEWEB)

    Washington, Aaron L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Narrows, William [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Christian, Jonathan H. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Msgwood, Leroy [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-07-27

    During Decommissioning and Demolition (D&D) activities at SRS, it is important that the building be screened for radionuclides and heavy metals to ensure that the proper safety and disposal metrics are in place. A major source of contamination at DOE facilities is the accumulation of mercury contamination, from nuclear material processing and Liquid Waste System (LWS). This buildup of mercury could possibly cause harm to any demolition crew or the environment should this material be released. The current standard method is to take core samples in various places in the facility and use X-ray fluorescence (XRF) to detect the contamination. This standard method comes with a high financial value due to the security levels of these sample facilities with unknown contamination levels. Here in we propose the use of portable XRF units to detect for this contamination on-site. To validate this method, the instrument has to be calibrated to detect the heavy metal contamination, be both precise with the known elemental concentrations and consistent with its actual results of a sample concrete and pristine contaminant, and be able to detect changes in the sample concrete’s composition. After receiving the various concrete samples with their compositions found by a XRF wave-dispersive method, the calibration factor’s linear regressions were adjusted to give the baseline concentration of the concrete with no contamination. Samples of both concrete and concrete/flyash were evaluated; their standard deviations revealed that the measurements were consistent with the known composition. Finally, the samples were contaminated with different concentrations of sodium tungsten dihydrate, allowed to air dry, and measured. When the contaminated samples were analyzed, the heavy metal contamination was seen within the spectrum of the instrument, but there was not a trend of quantification based on the concentration of the solution.

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

    Directory of Open Access Journals (Sweden)

    Robert A Colvin

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-06-15

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

  19. A correlation of breast cancer and calcium levels in hair analyzed by X-ray fluorescence.

    Science.gov (United States)

    Chikawa, Jun-ichi; Mouri, Yoshitaka; Shima, Hiroki; Yamada, Kousaku; Yamamoto, Hitoshi; Yamamoto, Shingo

    2014-01-01

    Time variations of elemental concentrations and their abnormalities due to breast cancer have been observed along single hair strands by X-ray fluorescence excited by synchrotron radiation. The renal-controlled elements Ca, Sr, S, K, Cl, Br and P have upper and lower levels associated with gating and closing of ion channels in the hair-making cells. The Ca lower level is normal. In cases of Ca deficiency, with a decrease from the normal, store-operated Ca channel gating occurs so as to keep the hair Ca at the normal, and paradoxically high Ca levels near or at the upper level are produced by PTH-operated channel gating of the cells. Chronic Ca deficiency shows a temporal pattern along the hair consisting of a long-term duration of the upper [Ca] level, 10-month long decay to the lower level and abrupt increase to the upper level. The observation for hair from breast-cancer patients also shows the upper Ca level for the time period well before detection, and suggests that cancer is always generated at the long-lasting [Ca] upper level and the hair [Ca] decreases gradually toward the lower level with the cancer growth. This decay of [Ca] is accompanied by those of [Sr] and [K]. Their different decay forms can be explained by parathyroid hormone related peptide (PTHrP) in serum secreted from the cancer having 150 times longer dwell time on the PTH receptors than that of PTH. Patient hair has a memory for the entire cancer process from the state before cancer generation, and the pattern can be distinguished from concentration variation due to the chronic Ca deficiency without cancer, leading to a criterion for cancer detection by the ratio of [Sr]/[Ca]. The hair analysis is useful for early detection of cancer.

  20. X-ray fluorescence microscopic measurement of elemental distribution in the mouse retina with age.

    Science.gov (United States)

    Grubman, Alexandra; Guennel, Philipp; Vessey, Kirstan A; Jones, Michael W M; James, Simon A; de Jonge, Martin D; White, Anthony R; Fletcher, Erica L

    2016-10-01

    The biologically important metals such as zinc, copper and iron play key roles in retinal function, yet no study has mapped the spatio-temporal distribution of retinal biometals in healthy or diseased retina. We investigated a natural mouse model of retinal degeneration, the Cln6nclf mouse. As dysfunctional metabolism of biometals is observed in the brains of these animals and deregulated metal homeostasis has been linked to retinal degeneration, we focused on mapping the elemental distribution in the healthy and Cln6nclf mouse retina with age. Retinal and RPE elemental homeostasis was mapped in Cln6nclf and C57BL6/J mice from 1 to 8 months of age using X-ray Fluorescence Microscopy at the Australian Synchrotron. In the healthy retina, we detected a progressive loss of phosphorus in the outer nuclear layer and significant reduction in iron in the inner segments of the photoreceptors. Further investigation revealed a unique elemental signature for each retinal layer, with high areal concentrations of iron and sulfur in the photoreceptor segments and calcium, phosphorus, zinc and potassium enrichment predominantly in the nuclear layers. The analysis of retinae from Cln6nclf mice did not show significant temporal changes in elemental distributions compared to age matched controls, despite significant photoreceptor cell loss. Our data therefore demonstrates that retinal layers have unique elemental composition. Elemental distribution is, with few exceptions, stably maintained over time in healthy and Cln6nclf mouse retina, suggesting conservation of elemental distribution is critical for basic retinal function with age and is not modulated by processes underlying retinal degeneration.

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

    Energy Technology Data Exchange (ETDEWEB)

    Wheeler, B.D.

    1999-07-01

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

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

    Directory of Open Access Journals (Sweden)

    Gregory Robison

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

  3. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

    Science.gov (United States)

    Ferretti, M.; Cristoforetti, G.; Legnaioli, S.; Palleschi, V.; Salvetti, A.; Tognoni, E.; Console, E.; Palaia, P.

    2007-12-01

    This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

  4. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Ferretti, M. [Istituto per le Tecnologie Applicate ai Beni Culturali, Via Salaria, km 29.300, c.p.10, 00016 Monterotondo St. - Roma (Italy); Cristoforetti, G.; Legnaioli, S. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Palleschi, V. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Salvetti, A.; Tognoni, E. [Applied Laser Spectroscopy Laboratory, Istituto per i Processi Chimico Fisici del CNR, Area di Ricerca di Pisa, Via G.Moruzzi, 1-56124 Pisa (Italy); Console, E. [T.E.A. s.a.s., Via Luigi Pascali, 23/25-88100 Catanzaro (Italy)], E-mail: elena@teacz.191.it; Palaia, P. [T.E.A. s.a.s., Via Luigi Pascali, 23/25-88100 Catanzaro (Italy)

    2007-12-15

    This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

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

    Science.gov (United States)

    Martin, Ronald Richard; Naftel, Steven; Macfie, Sheila; Jones, Keith; Nelson, Andrew

    2013-04-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-12-15

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

  7. Elemental analysis with a full-field X-ray fluorescence microscope and a CCD photon-counting system.

    Science.gov (United States)

    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.

  8. Rapid identification of polystyrene foam wastes containing hexabromocyclododecane or its alternative polymeric brominated flame retardant by X-ray fluorescence spectroscopy.

    Science.gov (United States)

    Schlummer, Martin; Vogelsang, Jörg; Fiedler, Dominik; Gruber, Ludwig; Wolz, Gerd

    2015-07-01

    The brominated flame retardant hexabromocyclododecane (HBCDD) was added to Annex A of the list of persistent organic pollutants (POPs) of the Stockholm Convention. Thus, production and use of HBCDD will be banned, and the recycling of HBCDD-containing foam waste will be restricted. In reaction a special polymeric brominated flame retardant (PolyFR) was developed to replace HBCDD in expanded and extruded polystyrene foams for building and construction applications. A decision has to be made at some future time whether expanded and extruded polystyrene foam waste is to be subjected to incineration (with HBCDD) or to recycling (without HBCDD). Therefore, an appropriate and rapid field method is required to distinguish between foams containing HBCDD and foams free from HBCDD. Here we present a screening method for identifying HBCDD containing expanded and extruded polystyrene foams. The test principle is based on the fact that PolyFR (a brominated polymeric macromolecule) is not extractable whereas HBCDD (a low molecular weight substance) is extractable. Following rapid extraction of HBCDD the brominated flame retardant is identified and quantified via bromine analysis using a handheld X-ray fluorescence instrument. The method was applied successfully to 27 expanded and extruded polystyrene foam samples (foams and extruded polystyrene foam raw materials), which were provided without any information about the applied flame retardant. The presence of HBCDD was confirmed for all HBCDD-positive samples in the test. A robustness test revealed a high degree of correctness and a high repeatability for the test system: samples containing HBCDD and HBCDD-free samples were identified correctly with relative standard deviations of quantitative results below 14%. Moreover, X-ray fluorescence spectroscopy test results agree well with HBCDD determinations performed in a laboratory with a gas chromatograph coupled to a flame ionisation detector. © The Author(s) 2015.

  9. Study of heavy metals and other elements in macrophyte algae using energy-dispersive X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, M.L.; Amorim, P.; Marques, M.I.M.; Ramos, M.T. [Univ. de Lisboa (Portugal); Ferreira, J.G. [Faculdade de Ciencias e Tecnologia, Monte de Caparica (Portugal). Dept. Ciencias e Engenharia do Ambiente

    1997-04-01

    Fucus vesiculosus L. seaweeds from three estuarine stations were analyzed by X-ray fluorescence, providing results for the concentration of total K, Ca, Ti, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sr, and Pb. Four different structures of the algae (base, stipe, reproductive organs, and growing tips) were analyzed to study the differential accumulation of heavy metals by different parts of Fucus. Some elements (e.g., Cu and Fe) are preferentially accumulated in the base of the algae, whereas others (e.g., As) exhibit higher concentrations in the reproductive organs and growing tips. The pattern of accumulation in different structures is similar for Cu, Zn, and Pb, but for other metals there is considerable variability in accumulation between parts of the plant. This is important in determining which structures of the plant should be used for biomonitoring. For samples collected at stations subject to differing metal loads, the relative elemental composition is approximately constant, notwithstanding significant variation in absolute values. The proportion of metals in Fucus is similar to that found in other estuaries, where metal concentrations are significantly lower. Energy-dispersive X-ray fluorescence has been shown to be a suitable technique for multielement analysis in this type of sample. No chemical pretreatment is required, minimizing sample contamination. The small amount of sample required, and the wide range of elements that can be detected simultaneously make energy-dispersive X-ray fluorescence a valuable tool for pollution studies.

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

    Science.gov (United States)

    Ohata, Masaki; Kidokoro, Toshihiro; Hioki, Akiharu

    2012-01-01

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

  11. The Catalytic Conversion of Thiophenes over Large H-ZSM-5 Crystals: An X-Ray, UV/Vis, and Fluorescence Microspectroscopic Study

    NARCIS (Netherlands)

    Kox, M.H.F.; Mijovilovich, A.E.; S ättler, J.J.H.B.; Stavitski, I.; Weckhuysen, B.M.

    2013-01-01

    X-ray absorption, UV/Vis, and fluorescence microspectroscopy have been used to characterize the catalytic conversion of thiophene derivatives within the micropores of an individual H-ZSM-5 zeolite crystal. Space-resolved information into the Si/ Al ratios and sulfur content was provided by X-ray

  12. Combination of grazing incidence x-ray fluorescence with x-ray reflectivity in one table-top spectrometer for improved characterization of thin layer and implants on/in silicon wafers.

    Science.gov (United States)

    Ingerle, D; Schiebl, M; Streli, C; Wobrauschek, P

    2014-08-01

    As Grazing Incidence X-ray Fluorescence (GIXRF) analysis does not provide unambiguous results for the characterization of nanometre layers as well as nanometre depth profiles of implants in silicon wafers by its own, the approach of providing additional information using the signal from X-ray Reflectivity (XRR) was tested. As GIXRF already uses an X-ray beam impinging under grazing incidence and the variation of the angle of incidence, a GIXRF spectrometer was adapted with an XRR unit to obtain data from the angle dependent fluorescence radiation as well as data from the reflected beam. A θ-2θ goniometer was simulated by combining a translation and tilt movement of a Silicon Drift detector, which allows detecting the reflected beam over 5 orders of magnitude. HfO2 layers as well as As implants in Silicon wafers in the nanometre range were characterized using this new setup. A just recently published combined evaluation approach was used for data evaluation.

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

    Science.gov (United States)

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

    2015-04-01

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

  14. Using X-Ray Fluorescence Technique to Quantify Metal Concentration in Coral Cores from Belize

    Science.gov (United States)

    Kingsley, C.; Bhattacharya, A.; Hangsterfer, A.; Carilli, J.; Field, D. B.

    2016-12-01

    Caribbean coral reefs are some of the most threatened marine ecosystems in the world. Research appears to suggest that environmental stressors of local origin, such as sediment run off, can reduce the resilience of these reefs to global threats such as ocean warming. Sedimentation can stunt coral growth, reduce its resilience, and it is possible that trapped material could render coral skeletons brittle (personal discussions). Material trapped in coral skeletons can provide information on the sources of particulate matter in the ocean ecosystem. Despite the importance of quantifying sources and types of materials trapped in corals, the research community is yet to fully develop techniques that allow accurate representation of trapped matter, which is potentially a major source of metal content in reef building coral skeletons. The dataset presented here explores the usefulness of X-Ray Fluorescence (XRF), a widely used tool in environmental studies (but generally not in corals), to estimate metal content in coral cores collected from four locations near Belize, with varying degrees of impact from coastal processes. The coral cores together cover a period of 1862-2006. Trace, major, and minor metal content from these cores have been well-studied using solution-based ICP-MS, providing us with the unique opportunity to test the efficacy of XRF technique in characterizing metal content in these coral cores. We have measured more than 50 metals using XRF every two millimeters along slabs removed from the middle of a coral core to characterize materials present in coral skeletons. We compared the results from XRF to solution-based ICP-MS - that involves dissolving subsamples of coral skeleton to measure metal content. Overall, it appears that the non-destructive XRF technique is a viable supplement in determining sediment and metal content in coral cores, and may be particularly helpful for assessing resistant phases such as grains of sediment that are not fully

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-05-08

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-02-17

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

  17. Sampling and data-taking strategies in X-ray fluorescence assay of low S/N solutions

    Science.gov (United States)

    Hudgens, C. R.

    This projet was initiated for the purpose of demonstrating the feasibility of on-line X-ray fluorescence (XRF) analysis for the nondestructive assay of fissile elements (SNM) in reactor fuel reprocessing (dissolver) solutions, using wavelength dispersive X-ray fluorescence analysis because of its high immunity to the intense gamma emissions of the solutions. A prime objective of this project was the identification and dimensioning of the parameters critical to XRF assays of high accuracy. The concepts presented herein, though directed primarily to assay of solutions with emphasis on low signal-to-noise conditions and low count rates, are applicable to all assays of solids, slurries, and gases. This study shows that for solution analysis total sampling gives total mass assays with no need for solution density or tank volume measurements. Time savings and standard deviations are both benefited by systematically predetermining the count requirements of analysts, standards, and backgrounds by the use of equations based on propagation of error considerations. This becomes quite important when assaying dilute solutions, in which the signal-to-noise ratios of the X-ray intensities are very low. When counting times are long, short dwell times at each spectrometer setting significantly counteract error accumulation arising from long-term instrumental drift.

  18. Quantitative X-ray fluorescence computed tomography for low-Z samples using an iterative absorption correction algorithm

    Directory of Open Access Journals (Sweden)

    Rong Huang

    2017-05-01

    Full Text Available X-ray fluorescence computed tomography is often used to measure trace element distributions within low-Z samples, using algorithms capable of X-ray absorption correction when sample self-absorption is not negligible. Its reconstruction is more complicated compared to transmission tomography, and therefore not widely used. We describe in this paper a very practical iterative method that uses widely available transmission tomography reconstruction software for fluorescence tomography. With this method, sample self-absorption can be corrected not only for the absorption within the measured layer but also for the absorption by material beyond that layer. By combining tomography with analysis for scanning X-ray fluorescence microscopy, absolute concentrations of trace elements can be obtained. By using widely shared software, we not only minimized the coding, took advantage of computing efficiency of fast Fourier transform in transmission tomography software, but also thereby accessed well-developed data processing tools coming with well-known and reliable software packages. The convergence of the iterations was also carefully studied for fluorescence of different attenuation lengths. As an example, fish eye lenses could provide valuable information about fish life-history and endured environmental conditions. Given the lens’s spherical shape and sometimes the short distance from sample to detector for detecting low concentration trace elements, its tomography data are affected by absorption related to material beyond the measured layer but can be reconstructed well with our method. Fish eye lens tomography results are compared with sliced lens 2D fluorescence mapping with good agreement, and with tomography providing better spatial resolution.

  19. Quantitative X-ray fluorescence computed tomography for low-Z samples using an iterative absorption correction algorithm

    Science.gov (United States)

    Huang, Rong; Limburg, Karin; Rohtla, Mehis

    2017-05-01

    X-ray fluorescence computed tomography is often used to measure trace element distributions within low-Z samples, using algorithms capable of X-ray absorption correction when sample self-absorption is not negligible. Its reconstruction is more complicated compared to transmission tomography, and therefore not widely used. We describe in this paper a very practical iterative method that uses widely available transmission tomography reconstruction software for fluorescence tomography. With this method, sample self-absorption can be corrected not only for the absorption within the measured layer but also for the absorption by material beyond that layer. By combining tomography with analysis for scanning X-ray fluorescence microscopy, absolute concentrations of trace elements can be obtained. By using widely shared software, we not only minimized the coding, took advantage of computing efficiency of fast Fourier transform in transmission tomography software, but also thereby accessed well-developed data processing tools coming with well-known and reliable software packages. The convergence of the iterations was also carefully studied for fluorescence of different attenuation lengths. As an example, fish eye lenses could provide valuable information about fish life-history and endured environmental conditions. Given the lens's spherical shape and sometimes the short distance from sample to detector for detecting low concentration trace elements, its tomography data are affected by absorption related to material beyond the measured layer but can be reconstructed well with our method. Fish eye lens tomography results are compared with sliced lens 2D fluorescence mapping with good agreement, and with tomography providing better spatial resolution.

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

    CERN Document Server

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

    2002-01-01

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

  1. Energy-dispersive X-ray fluorescence study of elemental uptake in ...

    Indian Academy of Sciences (India)

    A109Cd radioisotope-induced energy-dispersive X-ray fluorescence (EDXRF) study has been performed on samples of cauliflower consisting of the flower, the leaves and the associated root soil. The cauliflowers were collected from farms near the main dumping site of municipal solid waste in the city of Kolkata, India and ...

  2. X-ray fluorescence study of organic-inorganic polymer conversion into ceramics induced by ion irradiation

    Science.gov (United States)

    Kurmaev, E. Z.; Moewes, A.; Krietemeyer, M.; Endo, K.; Ida, T.; Shimada, S.; Winarski, R. P.; Neumann, M.; Shamin, S. N.; Ederer, D. L.

    1999-12-01

    Changes to the local and electronic structures of phenyltriethoxysilane (PTES) films when irradiated at room temperature with gold ion concentrations of 5×1014 to 2.5×1015 cm-2 and with carbon ion concentrations of 5×1015 cm-2 were studied using x-ray emission and photoelectron spectroscopies. The fluorescent ultrasoft silicon LII,III and carbon Kα x-ray emission spectra of unirradiated and irradiated PTES films were measured at the Advanced Light Source, and the Center for Advanced Microstructures and Devices. It is found that the PTES polymers that are exposed to ion doses higher than 5×1014 cm-2 convert to Si:O:C ceramics. Annealing the irradiated PTES polymer films at 1000 °C segregates the carbon atoms into sp2-like clusters.

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

    Science.gov (United States)

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

    2013-01-01

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

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

    CERN Document Server

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

    2003-01-01

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

  5. Assessment of marine and urban-industrial environments influence on built heritage sandstone using X-ray fluorescence spectroscopy and complementary techniques

    Science.gov (United States)

    Morillas, Héctor; García-Galan, Javier; Maguregui, Maite; Marcaida, Iker; García-Florentino, Cristina; Carrero, Jose Antonio; Madariaga, Juan Manuel

    2016-09-01

    The sandstone used in the construction of the tower of La Galea Fortress (Getxo, north of Spain) shows a very bad conservation state and a high percentage of sandstone has been lost. The fortress is located just on a cliff and close to the sea, and it experiments the direct influence of marine aerosol and also the impact of acid gases (SOx and NOx) coming from the surrounding industry and maritime traffic. This environment seems to be very harmful for the preservation of the sandstone used in it, promoting different pathologies (disintegration, alveolization, cracking or erosion blistering, salts crystallization on the pores, efflorescences etc.). In this work, a multianalytical methodology based on a preliminary in-situ screening of the affected sandstone using a handheld energy dispersive X-ray fluorescence spectrometer (HH-ED-XRF) and a subsequent characterization of extracted sample in the laboratory using elemental (μ-ED-XRF, Scanning Electron Microscope coupled to an X-Max Energy-Dispersive (SEM-EDS) and Inductively coupled plasma mass spectrometry (ICP-MS)) and molecular techniques (micro-Raman spectroscopy (μ-RS) and X-ray Diffraction (XRD)) was applied in order to characterize the original composition of this kind of stone and related deterioration products. With the whole methodology, it was possible to assess that the sandstone contain a notable percentage of calcite. The sulfation and nitration of this carbonate detected in the stone led to the dissolution process of the sandstone, promoting the observed material loss. Additionally, the presence of salts related with the influence of marine aerosol confirms that this kind of environment have influence on the conservation state of the sandstone building.

  6. Quantification and localization of trace metals in natural plancton using a synchrotron x-ray fluorescence microprobe.

    Energy Technology Data Exchange (ETDEWEB)

    Twining, B. S.; Baines, S. B.; Fisher, N. S.; Jacobsen, C.; Maser, J.; State Univ. of New York at Stony Brook

    2003-03-01

    The accumulation of trace metals by planktonic protists influences the growth of primary producers, metal biogeochemical cycling, and metal bioaccumulation in aquatic food chains. Despite their importance, unequivocal measurements of trace element concentrations in individual plankton cells have not been possible to date. We have used the 2-ID-E side-branch hard x-ray microprobe at the Advanced Photon Source to measure trace elements in individual marine plankton cells. This microprobe employs zoneplate optics to produce the sub-micron spatial resolution and low background fluorescence required to produce trace element maps of planktonic protist cells ranging in size from 3 to >50 {micro}m. We have developed preservation, rinsing, and mounting protocols that remove most of the salt from our marine samples, thus simplifying the identification of unknown cells and reducing high Cl-related background fluorescence. We have also developed spectral modeling techniques that account for the frequent overlap of adjacent fluorescence peaks and non-uniform detector response. Finally, we have used parallel soft x-ray transmission and epifluorescence microscopy images to estimate C normalized trace element concentrations, identify functional cell types (e.g., photosynthetic vs. non-photosynthetic), and correlate cell structures with spatial patterns in trace element fluorescence.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-07-01

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

  8. A high-quality multilayer structure characterization method based on X-ray fluorescence and Monte Carlo simulation

    Energy Technology Data Exchange (ETDEWEB)

    Brunetti, Antonio; Golosio, Bruno [Universita degli Studi di Sassari, Dipartimento di Scienze Politiche, Scienze della Comunicazione e Ingegneria dell' Informazione, Sassari (Italy); Melis, Maria Grazia [Universita degli Studi di Sassari, Dipartimento di Storia, Scienze dell' Uomo e della Formazione, Sassari (Italy); Mura, Stefania [Universita degli Studi di Sassari, Dipartimento di Agraria e Nucleo di Ricerca sulla Desertificazione, Sassari (Italy)

    2014-11-08

    X-ray fluorescence (XRF) is a well known nondestructive technique. It is also applied to multilayer characterization, due to its possibility of estimating both composition and thickness of the layers. Several kinds of cultural heritage samples can be considered as a complex multilayer, such as paintings or decorated objects or some types of metallic samples. Furthermore, they often have rough surfaces and this makes a precise determination of the structure and composition harder. The standard quantitative XRF approach does not take into account this aspect. In this paper, we propose a novel approach based on a combined use of X-ray measurements performed with a polychromatic beam and Monte Carlo simulations. All the information contained in an X-ray spectrum is used. This approach allows obtaining a very good estimation of the sample contents both in terms of chemical elements and material thickness, and in this sense, represents an improvement of the possibility of XRF measurements. Some examples will be examined and discussed. (orig.)

  9. Application of the Monte Carlo method to the analysis of doses and shielding around an X-ray fluorescence equipment

    Directory of Open Access Journals (Sweden)

    Ródenas José

    2017-01-01

    Full Text Available An X-ray fluorescence equipment is used for practical exercises in the laboratory of Nuclear Engineering of the Polytechnic University of Valencia (Spain. This equipment includes a compact X-ray tube, ECLIPSE-III, and a Si–PIN XR-100T detector. The voltage (30 kV, and the current (100 μA of the tube are low enough so that expected doses around the tube do not represent a risk for students working in the laboratory. Nevertheless, doses and shielding should be evaluated to accomplish the ALARA criterion. The Monte Carlo method has been applied to evaluate the dose rate around the installation provided with a shielding composed by a box of methacrylate. Dose rates calculated are compared with experimental measurements to validate the model. Obtained results show that doses are below allowable limits. Hence, no extra shielding is required for the X-ray beam. A previous Monte Carlo model was also developed to obtain the tube spectrum and validated by comparison with data from manufacturer.

  10. Evaluation of the composition of filters additional of equipment radiological intraoral by energy dispersive x-ray fluorescence (EDXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Franca, Alana Caroline; Torres, Catarina A.M.P.; Rocha, Ana S.S.; Deniak, Valeriy; Lara, Alessandro L.; Paschuk, Sergei A., E-mail: alanacarolinef@gmail.com, E-mail: sergei@utfpr.edu.br [Universidade Tecnologica Federal do Parana (CPGEI/UTFPR), Curitiba, PR (Brazil). Programa de Pos-Graduacao em Engenharia Eletrica e Informatica Industrial; Fernandes, Angela; Westphalen, Fernando Henrique, E-mail: angelafernandes@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Setor de Ciencias da Saude

    2013-07-01

    The need for high quality standards for radiographic images in order to make a diagnosis assertive, and being the additional filtration required in the intraoral X-ray equipment show the need of evaluating these filters. This study aims to examine the influence of the elemental composition of the filters of X-ray of dental intraoral equipment in the radiographic images quality. The filters analysis were performed by using the energy dispersive X-ray fluorescence method (EDXRF). Ten conventional filters were analysed. In this study, 33 radiographic exposures were performed using films: twenty radiographs in the incisor region and ten in the molar region, three exposures were also made in the same regions with same conditions without using filter. After radiographs development, optical density was measure and all radiographs were submitted to subjective evaluation by dental radiologists. Data obtained were correlated to effects evaluation of the elemental composition of all filters in the quality of the radiographic images. The elements found were: aluminum, cobalt, copper, sulfur, iron, manganese, titanium, zinc, and zirconium. The images obtained were identified in groups: Molars to 0.3 s; Incisors to 0.2 s; Incisors to 0.3 s, and for the group without filters. From the results obtained it was concluded that both unclear radiographs and ideal radiographs were produced by using filters of elementary common. Therefore, conventional filters evaluated were an acceptable option to produce quality images in dental radiology, despite differences in the composition of the alloys. (author)

  11. Application of the Monte Carlo method to the analysis of doses and shielding around an X-ray fluorescence equipment

    Science.gov (United States)

    Ródenas, José; Juste, Belén; Gallardo, Sergio; Querol, Andrea

    2017-09-01

    An X-ray fluorescence equipment is used for practical exercises in the laboratory of Nuclear Engineering of the Polytechnic University of Valencia (Spain). This equipment includes a compact X-ray tube, ECLIPSE-III, and a Si-PIN XR-100T detector. The voltage (30 kV), and the current (100 μA) of the tube are low enough so that expected doses around the tube do not represent a risk for students working in the laboratory. Nevertheless, doses and shielding should be evaluated to accomplish the ALARA criterion. The Monte Carlo method has been applied to evaluate the dose rate around the installation provided with a shielding composed by a box of methacrylate. Dose rates calculated are compared with experimental measurements to validate the model. Obtained results show that doses are below allowable limits. Hence, no extra shielding is required for the X-ray beam. A previous Monte Carlo model was also developed to obtain the tube spectrum and validated by comparison with data from manufacturer.

  12. Engineering iodine-doped carbon dots as dual-modal probes for fluorescence and X-ray CT imaging

    Science.gov (United States)

    Zhang, Miaomiao; Ju, Huixiang; Zhang, Li; Sun, Mingzhong; Zhou, Zhongwei; Dai, Zhenyu; Zhang, Lirong; Gong, Aihua; Wu, Chaoyao; Du, Fengyi

    2015-01-01

    X-ray computed tomography (CT) is the most commonly used imaging technique for noninvasive diagnosis of disease. In order to improve tissue specificity and prevent adverse effects, we report the design and synthesis of iodine-doped carbon dots (I-doped CDs) as efficient CT contrast agents and fluorescence probe by a facile bottom-up hydrothermal carbonization process. The as-prepared I-doped CDs are monodispersed spherical nanoparticles (a diameter of ~2.7 nm) with favorable dispersibility and colloidal stability in water. The aqueous solution of I-doped CDs showed wavelength-dependent excitation and stable photoluminescence similar to traditional carbon quantum dots. Importantly, I-doped CDs displayed superior X-ray attenuation properties in vitro and excellent biocompatibility. After intravenous injection, I-doped CDs were distributed throughout the body and excreted by renal clearance. These findings validated that I-doped CDs with high X-ray attenuation potency and favorable photoluminescence show great promise for biomedical research and disease diagnosis. PMID:26609232

  13. Scanning X-ray fluorescent elemental microanalysis with synchrotron radiation in geochemical research

    Science.gov (United States)

    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

  14. Gadolinium Deposition in Nephrogenic Systemic Fibrosis: An Examination of Tissue using Synchrotron X-ray Fluorescence Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    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.

  15. X-ray Excited Optical Fluorescence and Diffraction Imaging of Reactivity and Crystallinity in a Zeolite Crystal: Crystallography and Molecular Spectroscopy in One.

    Science.gov (United States)

    Ristanović, Zoran; Hofmann, Jan P; Richard, Marie-Ingrid; Jiang, Tao; Chahine, Gilbert A; Schülli, Tobias U; Meirer, Florian; Weckhuysen, Bert M

    2016-06-20

    Structure-activity relationships in heterogeneous catalysis are challenging to be measured on a single-particle level. For the first time, one X-ray beam is used to determine the crystallographic structure and reactivity of a single zeolite crystal. The method generates μm-resolved X-ray diffraction (μ-XRD) and X-ray excited optical fluorescence (μ-XEOF) maps of the crystallinity and Brønsted reactivity of a zeolite crystal previously reacted with a styrene probe molecule. The local gradients in chemical reactivity (derived from μ-XEOF) were correlated with local crystallinity and framework Al content, determined by μ-XRD. Two distinctly different types of fluorescent species formed selectively, depending on the local zeolite crystallinity. The results illustrate the potential of this approach to resolve the crystallographic structure of a porous material and its reactivity in one experiment via X-ray induced fluorescence of organic molecules formed at the reactive centers.

  16. Correlative cryo-fluorescence and cryo-soft X-ray tomography of adherent cells at European synchrotrons.

    Science.gov (United States)

    Carzaniga, Raffaella; Domart, Marie-Charlotte; Duke, Elizabeth; Collinson, Lucy M

    2014-01-01

    Cryo-soft X-ray tomography (cryo-SXT) is a synchrotron-hosted imaging technique used to analyze the ultrastructure of intact, cryo-prepared cells. Correlation of cryo-fluorescence microscopy and cryo-SXT can be used to localize fluorescent proteins to organelles preserved close to native state. Cryo-correlative light and X-ray microscopy (cryo-CLXM) is particularly useful for the study of organelles that are susceptible to chemical fixation artifacts during sample preparation for electron microscopy. In our recent work, we used cryo-CLXM to characterize GFP-LC3-positive early autophagosomes in nutrient-starved HEK293A cells (Duke et al., 2013). Cup-shaped omegasomes were found to form at "hot-spots" on the endoplasmic reticulum. Furthermore, cryo-SXT image stacks revealed the presence of large complex networks of tubulated mitochondria in the starved cells, which would be challenging to model at this scale and resolution using light or electron microscopy. In this chapter, we detail the cryo-CLXM workflow that we developed and optimized for studying adherent mammalian cells. We show examples of data collected at the three European synchrotrons that currently host cryo-SXT microscopes, and describe how raw cryo-SXT datasets are processed into tomoX stacks, modeled, and correlated with cryo-fluorescence data to identify structures of interest. © 2014 Elsevier Inc. All rights reserved.

  17. X-ray fluorescence - a non-destructive tool in investigation of Czech fine and applied art objects

    Science.gov (United States)

    Trojek, T.; Musílek, L.

    2017-08-01

    A brief review of application of X-ray fluorescence analysis (XRFA) to fine and applied arts related to Czech cultural heritage is presented. The Department of Dosimetry and Application of Ionising Radiation of CTU-FNSPE has used XRFA in collaboration with various Czech institutions dealing with cultural history for many kinds of artefacts, (e.g., Roman and medieval brass, gemstones and noble metals from the sceptre of one of the faculties of the Charles University in Prague, millefiori beads, etc.). In some cases, a combination of various other techniques alongside XRFA was used for enhancing our knowledge of a measured object.

  18. In situ multi-element analyses by energy-dispersive X-ray fluorescence on varnishes of historical violins

    Energy Technology Data Exchange (ETDEWEB)

    Echard, Jean-Philippe [Laboratoire de recherche et de restauration, Musee de la musique, Cite de la musique, 221, avenue Jean-Jaures, 75019 Paris (France)]. E-mail: jpechard@cite-musique.fr

    2004-10-08

    Varnishes of Italian violins and other historical stringed instruments have been analyzed by energy-dispersive X-ray fluorescence (EDXRF). The instruments whose varnishes were to be analyzed were chosen from the collection kept in Musee de la Musique in Paris. Direct analyses were performed on instrument varnishes, without any sampling and non-destructively, showing inorganic elements such as lead, mercury and iron that could be related to siccatives or pigments. Analytical results and their comparison with old formulae or traditional recipes of violin varnishes, as with the few previous analytical results, will be discussed.

  19. Use of portable X-ray fluorescence spectrometry for environmental quality assessment of peri-urban agriculture.

    Science.gov (United States)

    Weindorf, David C; Zhu, Yuanda; Chakraborty, Somsubhra; Bakr, Noura; Huang, Biao

    2012-01-01

    Urban expansion into traditional agricultural lands has augmented the potential for heavy metal contamination of soils. This study examined the utility of field portable X-ray fluorescence (PXRF) spectrometry for evaluating the environmental quality of sugarcane fields near two industrial complexes in Louisiana, USA. Results indicated that PXRF provided quality results of heavy metal levels comparable to traditional laboratory analysis. When coupled with global positioning system technology, the use of PXRF allows for on-site interpolation of heavy metal levels in a matter of minutes. Field portable XRF was shown to be an effective tool for rapid assessment of heavy metals in soils of peri-urban agricultural areas.

  20. Energy Dispersive X-Ray Fluorescent Analysis of Soil in the Vicinity of Industrial Areas and Heavy Metal Pollution Assessment

    Science.gov (United States)

    Singh, V.; Joshi, G. C.; Bisht, D.

    2017-05-01

    The soil of two agricultural sites near an industrial area was investigated for heavy metal pollution using energy dispersive X-ray fluorescence (EDXRF). The concentration values for 17 elements were determined in the soil samples including eight heavy metal elements, i.e., Fe, Ni, As, Pb, Mn, Cr, Cu, and Zn. The soil near a pulp and paper mill was found to be highly polluted by the heavy metals. The concentration data obtained by EDXRF were further examined by calculating the pollution index and Nemerow integrated pollution index.

  1. Detection of metallic elements from paraffin-embedded tissue blocks by energy dispersive X-ray fluorescence spectrometry.

    Science.gov (United States)

    Takahashi, Motonori; Kinoshita, Hiroshi; Nishiguchi, Minori; Nishio, Hajime

    2010-03-01

    Energy dispersive X-ray fluorescence spectrometry (EDX) enables rapid, non-destructive, multi-elemental analysis. Using EDX, lead and some other metallic elements were detected in paraffin-blocks in which skin samples from a gunshot wound were embedded. Lead was not identified in control samples from non-injured cases. These findings indicate that EDX is a useful method for rapid non-destructive analysis of paraffin-embedded blocks. This technique can provide scientific evidence for identification of a firearm even after storing the sample for a long time. (c) 2009 Elsevier Ireland Ltd. All rights reserved.

  2. Automatic reduction of large X-ray fluorescence data-sets applied to XAS and mapping experiments

    Energy Technology Data Exchange (ETDEWEB)

    Martin Montoya, Ligia Andrea

    2017-02-15

    In this thesis two automatic methods for the reduction of large fluorescence data sets are presented. The first method is proposed in the framework of BioXAS experiments. The challenge of this experiment is to deal with samples in ultra dilute concentrations where the signal-to-background ratio is low. The experiment is performed in fluorescence mode X-ray absorption spectroscopy with a 100 pixel high-purity Ge detector. The first step consists on reducing 100 fluorescence spectra into one. In this step, outliers are identified by means of the shot noise. Furthermore, a fitting routine which model includes Gaussian functions for the fluorescence lines and exponentially modified Gaussian (EMG) functions for the scattering lines (with long tails at lower energies) is proposed to extract the line of interest from the fluorescence spectrum. Additionally, the fitting model has an EMG function for each scattering line (elastic and inelastic) at incident energies where they start to be discerned. At these energies, the data reduction is done per detector column to include the angular dependence of scattering. In the second part of this thesis, an automatic method for texts separation on palimpsests is presented. Scanning X-ray fluorescence is performed on the parchment, where a spectrum per scanned point is collected. Within this method, each spectrum is treated as a vector forming a basis which is to be transformed so that the basis vectors are the spectra of each ink. Principal Component Analysis is employed as an initial guess of the seek basis. This basis is further transformed by means of an optimization routine that maximizes the contrast and minimizes the non-negative entries in the spectra. The method is tested on original and self made palimpsests.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-06-15

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

  4. A bench-top K X-ray fluorescence system for quantitative measurement of gold nanoparticles for biological sample diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Ricketts, K., E-mail: k.ricketts@ucl.ac.uk [Division of Surgery and Interventional Sciences, University College London, Royal Free Campus, Rowland Hill Street, London NW3 2PF (United Kingdom); Guazzoni, C.; Castoldi, A. [Dipartimento di Elettronica, Informazione e Bioingegneria Politecnico di Milano and INFN, Sezione di Milano P.za Leonardo da Vinci, 32-20133 Milano (Italy); Royle, G. [Department of Medical Physics and Bioengineering, University College London, Malet Place Engineering Building, Gower Street, London WC1E 6BT (United Kingdom)

    2016-04-21

    Gold nanoparticles can be targeted to biomarkers to give functional information on a range of tumour characteristics. X-ray fluorescence (XRF) techniques offer potential quantitative measurement of the distribution of such heavy metal nanoparticles. Biologists are developing 3D tissue engineered cellular models on the centimetre scale to optimise targeting techniques of nanoparticles to a range of tumour characteristics. Here we present a high energy bench-top K-X-ray fluorescence system designed for sensitivity to bulk measurement of gold nanoparticle concentration for intended use in such thick biological samples. Previous work has demonstrated use of a L-XRF system in measuring gold concentrations but being a low energy technique it is restricted to thin samples or superficial tumours. The presented system comprised a high purity germanium detector and filtered tungsten X-ray source, capable of quantitative measurement of gold nanoparticle concentration of thicker samples. The developed system achieved a measured detection limit of between 0.2 and 0.6 mgAu/ml, meeting specifications of biologists and being approximately one order of magnitude better than the detection limit of alternative K-XRF nanoparticle detection techniques. The scatter-corrected K-XRF signal of gold was linear with GNP concentrations down to the detection limit, thus demonstrating potential in GNP concentration quantification. The K-XRF system demonstrated between 5 and 9 times less sensitivity than a previous L-XRF bench-top system, due to a fundamental limitation of lower photoelectric interaction probabilities at higher K-edge energies. Importantly, the K-XRF technique is however less affected by overlying thickness, and so offers future potential in interrogating thick biological samples.

  5. High-Energy Resolution Fluorescence Detected X-Ray Absorption Spectroscopy: A Powerful New Structural Tool in Environmental Biogeochemistry Sciences.

    Science.gov (United States)

    Proux, Olivier; Lahera, Eric; Del Net, William; Kieffer, Isabelle; Rovezzi, Mauro; Testemale, Denis; Irar, Mohammed; Thomas, Sara; Aguilar-Tapia, Antonio; Bazarkina, Elena F; Prat, Alain; Tella, Marie; Auffan, Mélanie; Rose, Jérôme; Hazemann, Jean-Louis

    2017-11-01

    The study of the speciation of highly diluted elements by X-ray absorption spectroscopy (XAS) is extremely challenging, especially in environmental biogeochemistry sciences. Here we present an innovative synchrotron spectroscopy technique: high-energy resolution fluorescence detected XAS (HERFD-XAS). With this approach, measurement of the XAS signal in fluorescence mode using a crystal analyzer spectrometer with a ∼1-eV energy resolution helps to overcome restrictions on sample concentrations that can be typically measured with a solid-state detector. We briefly describe the method, from both an instrumental and spectroscopic point of view, and emphasize the effects of energy resolution on the XAS measurements. We then illustrate the positive impact of this technique in terms of detection limit with two examples dealing with Ce in ecologically relevant organisms and with Hg species in natural environments. The sharp and well-marked features of the HERFD-X-ray absorption near-edge structure spectra obtained enable us to determine unambiguously and with greater precision the speciation of the probed elements. This is a major technological advance, with strong benefits for the study of highly diluted elements using XAS. It also opens new possibilities to explore the speciation of a target chemical element at natural concentration levels, which is critical in the fields of environmental and biogeochemistry sciences. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  6. FMT-PCCT: hybrid fluorescence molecular tomography-x-ray phase-contrast CT imaging of mouse models.

    Science.gov (United States)

    Mohajerani, Pouyan; Hipp, Alexander; Willner, Marian; Marschner, Mathias; Trajkovic-Arsic, Marija; Ma, Xiaopeng; Burton, Neal C; Klemm, Uwe; Radrich, Karin; Ermolayev, Vladimir; Tzoumas, Stratis; Siveke, Jens T; Bech, Martin; Pfeiffer, Franz; Ntziachristos, Vasilis

    2014-07-01

    The implementation of hybrid fluorescence molecular tomography (FMT) and X-ray computed tomography (CT) has been shown to be a necessary development, not only for combining anatomical with functional and molecular contrast, but also for generating optical images of high accuracy. FMT affords highly sensitive 3-D imaging of fluorescence bio-distribution, but in stand-alone form it offers images of low resolution. It was shown that FMT accuracy significantly improves by considering anatomical priors from CT. Conversely, CT generally suffers from low soft tissue contrast. Therefore utilization of CT data as prior information in FMT inversion is challenging when different internal organs are not clearly differentiated. Instead, we combined herein FMT with emerging X-ray phase-contrast CT (PCCT). PCCT relies on phase shift differences in tissue to achieve soft tissue contrast superior to conventional CT. We demonstrate for the first time FMT-PCCT imaging of different animal models, where FMT and PCCT scans were performed in vivo and ex vivo, respectively. The results show that FMT-PCCT expands the potential of FMT in imaging lesions with otherwise low or no CT contrast, while retaining the cost benefits of CT and simplicity of hybrid device realizations. The results point to the most accurate FMT performance to date.

  7. Combined use of X-ray fluorescence microscopy, phase contrast imaging for high resolution quantitative iron mapping in inflamed cells

    Science.gov (United States)

    Gramaccioni, C.; Procopio, A.; Farruggia, G.; Malucelli, E.; Iotti, S.; Notargiacomo, A.; Fratini, M.; Yang, Y.; Pacureanu, A.; Cloetens, P.; Bohic, S.; Massimi, L.; Cutone, A.; Valenti, P.; Rosa, L.; Berlutti, F.; Lagomarsino, S.

    2017-06-01

    X-ray fluorescence microscopy (XRFM) is a powerful technique to detect and localize elements in cells. To derive information useful for biology and medicine, it is essential not only to localize, but also to map quantitatively the element concentration. Here we applied quantitative XRFM to iron in phagocytic cells. Iron, a primary component of living cells, can become toxic when present in excess. In human fluids, free iron is maintained at 10-18 M concentration thanks to iron binding proteins as lactoferrin (Lf). The iron homeostasis, involving the physiological ratio of iron between tissues/secretions and blood, is strictly regulated by ferroportin, the sole protein able to export iron from cells to blood. Inflammatory processes induced by lipopolysaccharide (LPS) or bacterial pathoge inhibit ferroportin synthesis in epithelial and phagocytic cells thus hindering iron export, increasing intracellular iron and bacterial multiplication. In this respect, Lf is emerging as an important regulator of both iron and inflammatory homeostasis. Here we studied phagocytic cells inflamed by bacterial LPS and untreated or treated with milk derived bovine Lf. Quantitative mapping of iron concentration and mass fraction at high spatial resolution is obtained combining X-ray fluorescence microscopy, atomic force microscopy and synchrotron phase contrast imaging.

  8. Prediction of Ba, Co and Ni for tropical soils using diffuse reflectance spectroscopy and X-ray fluorescence spectroscopy

    Science.gov (United States)

    Arantes Camargo, Livia; Marques Júnior, José; Reynaldo Ferracciú Alleoni, Luís; Tadeu Pereira, Gener; De Bortoli Teixeira, Daniel; Santos Rabelo de Souza Bahia, Angélica

    2017-04-01

    Environmental impact assessments may be assisted by spatial characterization of potentially toxic elements (PTEs). Diffuse reflectance spectroscopy (DRS) and X-ray fluorescence spectroscopy (XRF) are rapid, non-destructive, low-cost, prediction tools for a simultaneous characterization of different soil attributes. Although low concentrations of PTEs might preclude the observation of spectral features, their contents can be predicted using spectroscopy by exploring the existing relationship between the PTEs and soil attributes with spectral features. This study aimed to evaluate, in three geomorphic surfaces of Oxisols, the capacity for predicting PTEs (Ba, Co, and Ni) and their spatial variability by means of diffuse reflectance spectroscopy (DRS) and X-ray fluorescence spectroscopy (XRF). For that, soil samples were collected from three geomorphic surfaces and analyzed for chemical, physical, and mineralogical properties, and then analyzed in DRS (visible + near infrared - VIS+NIR and medium infrared - MIR) and XRF equipment. PTE prediction models were calibrated using partial least squares regression (PLSR). PTE spatial distribution maps were built using the values calculated by the calibrated models that reached the best accuracy using geostatistics. PTE prediction models were satisfactorily calibrated using MIR DRS for Ba, and Co (residual prediction deviation - RPD > 3.0), Vis DRS for Ni (RPD > 2.0) and FRX for all the studied PTEs (RPD > 1.8). DRS- and XRF-predicted values allowed the characterization and the understanding of spatial variability of the studied PTEs.

  9. Metal-binding proteins scanning and determination by combining gel electrophoresis, synchrotron radiation X-ray fluorescence and atomic spectrometry.

    Science.gov (United States)

    Verbi, F M; Arruda, S C C; Rodriguez, A P M; Pérez, C A; Arruda, M A Z

    2005-02-28

    In the present work, protein bands from in vitro embriogenic callus (Citrus sinensis L. Osbeck) were investigated using micro-synchrotron radiation X-ray fluorescence (muSR-XRF) after sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) separation. Metal-binding protein quantification was done after microwave oven decomposition of gel by synchrotron radiation total reflection X-ray fluorescence (SR-TXRF), flame atomic absorption spectrometry (FAAS) and flame atomic emission spectrometry (FAES). According to the analysis of the protein bands, it is possible to observe that both 81 and ca. 14 kDa proteins present different Fe signal intensity at different positions. The analysis of 53 kDa protein, showed even more interesting results. Besides Fe, the muSR-XRF experiments indicate the presence of Ca, Cu, K and Zn. Chemical elements such as Cu, K, Fe and Zn were determined by SR-TXRF, Mg by FAAS and Na by FAES. Ca was determined by SR-TXRF and FAAS only for accuracy check. In the mineralised protein bands of 81 and around 14 kDa band, only Fe was determined (105 and 21.8 microg g(-1)). For those protein bands (86-ca. 14 kDa) were determined, Ca, K, Cu and Zn in a wide concentration range (42.4-283, 2.47-96.8, 0.91-15.9 and 3.39-29.7 microg g(-1), respectively).

  10. Quarry identification of historical building materials by means of laser induced breakdown spectroscopy, X-ray fluorescence and chemometric analysis

    Science.gov (United States)

    Colao, F.; Fantoni, R.; Ortiz, P.; Vazquez, M. A.; Martin, J. M.; Ortiz, R.; Idris, N.

    2010-08-01

    To characterize historical building materials according to the geographic origin of the quarries from which they have been mined, the relative content of major and trace elements were determined by means of Laser Induced Breakdown Spectroscopy (LIBS) and X-ray Fluorescence (XRF) techniques. 48 different specimens were studied and the entire samples' set was divided in two different groups: the first, used as reference set, was composed by samples mined from eight different quarries located in Seville province; the second group was composed by specimens of unknown provenance collected in several historical buildings and churches in the city of Seville. Data reduction and analysis on laser induced breakdown spectroscopy and X-ray fluorescence measurements was performed using multivariate statistical approach, namely the Linear Discriminant Analysis (LDA), Principal Component Analysis (PCA) and Soft Independent Modeling of Class Analogy (SIMCA). A clear separation among reference sample materials mined from different quarries was observed in Principal Components (PC) score plots, then a supervised soft independent modeling of class analogy classification was trained and run, aiming to assess the provenance of unknown samples according to their elemental content. The obtained results were compared with the provenance assignments made on the basis of petrographical description. This work gives experimental evidence that laser induced breakdown spectroscopy measurements on a relatively small set of elements is a fast and effective method for the purpose of origin identification.

  11. Application of 'direct' beta particle excitation for the determination of noble metals in catalysts by radioisotope excited X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    LaBrecque, J.J.; Rosales, P.A.; Quiero, A. (Instituto Venezolano de Investigaciones Cientificas, Caracas)

    1982-01-01

    A new technique was applied for exciting X-rays for X-ray fluorescence analysis by 'direct' beta excitation for the determination of noble metals in catalytic materials. A series of five synthetic standards were prepared each for platinum and palladium in the range of 0.5-10% for both carbon and alumina supports. The X-ray spectrometer system employed was a modified TN-11 and /sup 147/Pm inserted directly in the sample itself acts as the excitation source. The detector was a high resolution Si(Li) semiconductor with better than 160 eV resolution.

  12. Simple procedure for nutrient analysis of coffee plant with energy dispersive X-ray fluorescence spectrometry (EDXRF)

    Energy Technology Data Exchange (ETDEWEB)

    Tezotto, Tiago; Favarin, Jose Laercio; Neto, Ana Paula; Azevedo, Ricardo Antunes, E-mail: tiago.tezotto@usp.br [Escola Superior de Agricultura Luiz de Queiroz (ESALQ/USP), Piracicaba, SP (Brazil); Gratao, Priscila Lupino [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP/ FCAV), Jaboticabal, SP (Brazil). Dept. de Biologia Aplicada a Agropecuaria; Mazzafera, Paulo [Universidade Estadual de Campinas (UNICAMP/IB), SP (Brazil). Dept. Biologia Vegetal

    2013-07-15

    Nutrient analysis is used to estimate nutrient content of crop plants to manage fertilizer application for sustained crop production. Direct solid analysis of agricultural and environmental samples by energy dispersive X-ray fluorescence spectrometry (EDXRF) was chosen as alternative technique to evaluate the simultaneous multielemental quantification of the most important essential elements in coffee (Coffea arabica L.) plants. Inductively coupled plasma atomic emission spectrometry and certified reference materials made from leaves were used to calibrate and check the trueness of EDXRF method for the determination of the concentration of several nutrients in coffee leaves and branches. Fluorescence spectrometry proved to be advantageous and presented low cost as loose powder samples could be used. Samples collected from a field experiment where coffee plants were treated with excess of Ni and Zn were used to verify the practical application of the method. Good relationships were achieved between certified values and data obtained by EDXRF, with recoveries ranging from 82 to 117 %.(author)

  13. Investigation of mineral distribution in bone by synchrotron X-ray fluorescence microscopy after tibolone therapy

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Rio de Janeiro State Univ., Nova Friburgo, RJ (Brazil). Dept. of Mechanical Engineering and Energy; Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Carvalho, A.C.B.; Henriques, H.N.; Guzman-Silva, M.A. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Lab. of Experimental Pathology; Sales, E.; Lopes, R.T. [Federal Univ. of Rio de Janeiro, RJ (Brazil). Nuclear Instrumentation Lab. - COPPE; Granjeiro, J.M. [Fluminense Federal Univ., Niteroi, RJ (Brazil). Dept. of Cellular and Molecular Biology

    2011-07-01

    Tibolone is a synthetic steroid with estrogenic, androgenic, and progestagenic properties used for the prevention of postmenopausal osteoporosis and treatment of climacteric symptoms. Tibolone shows almost no action on breast and endometrium, which are target-organs for estrogens and progesterone activity. The aim of this work was to investigate the spatial distribution of calcium and zinc minerals in the femoral head of ovariectomized rat in order to evaluate the effects of the long-term administration of tibolone. For that purpose X-ray microfluorescence was used with synchrotron radiation imaging technique which was performed at Brazilian Light Synchrotron Laboratory, Campinas, SP. Minerals were not homogeneously distributed in trabecular bone areas; a higher concentration of calcium in the trabecular regions at femoral heads was found in ovariectomized and tibolone-treated rats compared to ovariectomized and control groups. (orig.)

  14. Wavelength Dispersive X-ray Fluorescence Analysis of Actinides in Dissolved Nuclear Fuels

    Energy Technology Data Exchange (ETDEWEB)

    O' Hara, David [Parallax Research, Inc., Tallahassee, FL (United States)

    2015-10-15

    There is an urgent need for an instrument that can quickly measure the concentration of Plutonium and other Actinides mixed with Uranium in liquids containing dissolved spent fuel rods. Parallax Research, Inc. proposes to develop an x-ray spectrometer capable of measuring U, Np and Pu in dissolved nuclear fuel rod material to less than 10 ppm levels to aid in material process control for these nuclear materials. Due to system noise produced by high radioactivity, previous x-ray spectrometers were not capable of low level measurements but the system Parallax proposed has no direct path for undesired radiation to get to the detector and the detector in the proposed device is well shielded from scatter and has very low dark current. In addition, the proposed spectrometer could measure these three elements simultaneously, also measuring background positions with an energy resolution of roughly 100 eV making it possible to see a small amount of Pu that would be hidden under the tail of the U peak in energy dispersive spectrometers. Another nearly identical spectrometer could be used to target Am and Cm if necessary. The proposed spectrometer needs only a tiny sample of roughly 1 micro-liter (1 mm3) and the measurement can be done with the liquid flowing in a radiation and chemical immune quartz capillary protected by a stainless steel rod making it possible to continuously monitor the liquid or to use a capillary manifold to measure other liquid streams. Unlike other methods such as mass spectroscopy where the sample must be taken to a remote facility and might take days for turn-around, the proposed measurement should take less than an hour. This spectrometer could enable near real-time measurement of U, Pu and Np in dilute dissolved spent nuclear fuel rod streams.

  15. Estimation of Lead (Pb in Toys Using X-Ray Fluorescence Technology

    Directory of Open Access Journals (Sweden)

    Sandipayan Dutta

    2016-01-01

    Full Text Available Background: Lead exists extensively in the environment and it is a heavy metal, which is neurotoxic in nature which is harmful to children. In contrast to trace elements such as iron (Fe and zinc (Zn, lead has no recognized benecial effects in human body. With the economic development in India in recent years, the concentration of lead has increased in the environment and henceforth, lead pollution has become a severe problem in the country. Lead poisoning can create an immense damage and irreversible harm to foetal growth, the growth of teenagers and psychological, behavioural and cognitive development. Aim and Objectives: To estimate the lead content in the sample of toys. Material and Methods: 97 different toys were collected and coded as TS, these toys were kept in plastic lock cover which were lead proof. At rst the toys were arranged in order according to the serial number of the code (TS1 – TS97. The FP X-ray uorescence (Innov-X ray analyzer instrument was placed with the window of the analyzer on the surface of the toy vertically in such a way that there was no gap between the toy surface and the sampling window. The parts per million (ppm values of all toys were recorded. Results: Out of 97 samples tested, 22 samples were above permissible limits. The different materials demonstrate signicant correlation with the lead content in ppm. Lead is used as a stabilizer in some toys as well as children's items made from PVC plastic. Baby toys made up of plastic have higher concentration of lead. Lead can leach out of products when children handle and swallow them involuntarily.

  16. Quantitative Elemental Microanalysis Of Individual Particles With Use Of X-Ray Fluorescence Method And Monte Carlo Simulation

    Science.gov (United States)

    Czyzycki, Mateusz; Lankosz, Marek; Bielewski, Marek

    2010-04-01

    Recently a considerable interest has been triggered in the investigation of the composition of individual particles by X-ray fluorescence microanalysis. The sources of these micro-samples are mostly diversified. These samples come from space dust, air and ash, soil as well as environment and take the shape of a sphere or an oval. In analysis this kind of samples the geometrical effects caused by different sizes and shapes influence on accuracy of results. This fact arises from the matrix effect. For these samples it is not possible to find analytically a solution of equation taking into account an absorption of X-rays. Hence, a way out is to approximate the real sample shape with the other one or to use Monte Carlo (MC) simulation method. In current work authors utilized the iterative MC simulation to assess an elemental percentage of individual particles. The set of glass micro-spheres, made of NIST K3089 material of known chemical composition, with diameters in the range between 25 and 45 μm was investigated. The microspheres were scanned with X-ray tube primary radiation. Results of MC simulation were compared with these of some analytical approaches based on particle shape approximation. An investigation showed that the low-Z elements (Si, Ca, Ti) were the most sensitive on changes of particle shape and sizes. For high-Z elements (Fe—Pb) concentrations were nearly equal regardless of method used. However, for the all elements considered, results of MC simulation were more accurate then these of analytical relationships taken into comparison.

  17. Synchrotron radiation X-ray fluorescence microscopy reveals a spatial association of copper on elastic laminae in rat aortic media.

    Science.gov (United States)

    Qin, Zhenyu; Toursarkissian, Boulos; Lai, Barry

    2011-08-01

    Copper, an essential trace metal in humans, plays an important role in elastic formation. However, little is known about the spatial association between copper, elastin, and elastin producing cells. The aorta is the largest artery; the aortic media is primarily composed of the elastic lamellae and vascular smooth muscle cells, which makes it a good model to address this issue. Synchrotron radiation X-ray fluorescence microscopy (SRXRF) is a new generation technique to investigate the spatial topography of trace metals in biological samples. Recently, we utilized this technique to determine the topography of copper as well as other trace elements in aortic media of Sprague Dawley rats. A standard rat diet was used to feed Sprague Dawley rats, which contains the normal dietary requirements of copper and zinc. Paraffin embedded segments (4 μm of thickness) of thoracic aorta were analyzed using a 10 keV incident monochromatic X-ray beam focusing on a spot size of 0.3 μm × 0.2 μm (horizontal × vertical). The X-ray spectrum was measured using an energy-dispersive silicon drift detector for elemental topography. Our results showed that phosphorus, sulfur, and zinc are predominately distributed in the vascular smooth muscle cells, whereas copper is dramatically accumulated in elastic laminae, indicating a preferential spatial association of copper on elastic laminae in aortic media. This finding sheds new light on the role of copper in elastic formation. Our studies also demonstrate that SRXRF allows for the visualization of trace elements in tissues and cells of rodent aorta with high spatial resolution and provides an opportunity to study the role of trace elements in vasculature.

  18. An X-ray fluorescence microscopic analysis of the tissue surrounding the multi-channel cochlear implant electrode array.

    Science.gov (United States)

    Spiers, Kathryn; Cardamone, Tina; Furness, John B; Clark, Jonathan C M; Patrick, James F; Clark, Graeme M

    2016-05-01

    The aim of this study was to analyse the tissue surrounding the University of Melbourne's (UOMs) multi-channel cochlear implant electrode array and cochlear limited replacements, after long-term implantations. In particular, it aimed to identify the particulate material in the fibrous tissue capsule of the arrays implanted in 1978, 1983, and 1998, by using the Australian Synchrotron for X-ray fluorescence microscopy (XFM) to reveal the characteristic spectrum of metal, in particular platinum. This also helped to determine its format and chemical state. Tissue was retrieved following the recipient's death in 2007. Tissue was fixed and sections taken across the UOM and Cochlear Corporation (CI-22 and CI-24) electrode tracks. These were stained with Masson's trichrome. The Australian Synchrotron enabled XFM to accurately identify platinum from its characteristic fluorescence spectrum. There was a fibrous tissue capsule (about 100-µm thick) and small regions of calcification around the UOM and CI-22 arrays, but a thinner capsule (40-60-µm thick) around CI-24, and a greater degree of calcification. Dark particulate matter was observed within macrophages and especially in fibrous tissue in proximity to the UOM and CI-22 arrays. This was identified as platinum using X-ray fluorescence. There was also diffusion of platinum into the tissue surrounding the UOM and CI-22 electrodes and fine particles had penetrated the spiral ligament. The larger particulate matter in the tissue around the UOM and CI-22 arrays suggested that it had flaked off in the manufacturing of the UOM electrodes. The more diffuse spread of platinum in the tissue around the UOM and CI-22 electrodes was likely due to electrolysis, probably from charge imbalance with the bipolar pulses from the UOM implant. This did not occur with the Cochlear CI-24 device. Furthermore, the widespread fine particles of platinum could have also been due to corrosion, especially from the UOM electrodes.

  19. L X-ray fluorescence cross-sections of heavy elements excited by 16.04, 16.90 and 17.78 keV photons

    Energy Technology Data Exchange (ETDEWEB)

    Al-Saleh, K.A. [Department of Physics, University of Jordan, P.O. Box 13099, Amman (Jordan); Saleh, N.S. [Department of Physics, University of Jordan, P.O. Box 13099, Amman (Jordan)

    1999-01-01

    L{sub l}, L{sub {alpha}}, L{sub {beta}}, L{sub {gamma}} X-ray fluorescence cross sections have been measured for the elements Au, Pt, W, Lu, Yb, Tm, Ho, Dy and Tb using photon energies of 16.04, 16.90 and 17.78 keV. Measurements have been performed using an X-ray tube with a secondary-exciter system as an excitation source. The secondary exciters used are Zr, Nb and Mo of pure metal sheets (99.99%). A Mo X-ray tube with a secondary-target arrangement was used to obtain high intensity with a high degree of monochromaticity. Using an X-ray tube made it possible to measure X-ray fluorescence cross-sections and intensity ratios even for low intensity X-ray lines. The experimental values of the cross-sections were determined by measuring the absolute yield of L subshell X-rays emitted from a standard target of a given element irradiated with photons of given energy. The theoretical values of the cross-sections were calculated using theoretically tabulated values of subshell photoionization cross-sections, fluorescence yields, Coster-Kronig transition probabilities and radiative decay rates. Experimental results have been compared with the theoretically calculated values of L X-ray cross-sections. A fairly good agreement is observed between the experimental and the calculated values. The intensity ratios I{sub L{beta}}/I{sub L{alpha}} and I{sub L{gamma}}/I{sub L{alpha}} were measured and found to be in good agreement with the calculated values.

  20. Determination of selenium at trace levels in geologic materials by energy-dispersive X-ray fluorescence spectrometry

    Science.gov (United States)

    Wahlberg, J.S.

    1981-01-01

    Low levels of selenium (0.1-500 ppm) in both organic and inorganic geologic materials can be semiquantitatively measured by isolating Se as a thin film for presentation to an energy-dispersive X-ray fluorescence spectrometer. Suitably pulverized samples are first digested by fusing with a mixture of Na2CO3 and Na2O2. The fusion cake is dissolved in distilled water, buffered with NH4Cl, and filtered to remove Si and the R2O3 group. A carrier solution of Na2TeO4, plus solid KI, hydrazine sulfate and Na2SO3, is added to the filtrate. The solution is then vacuum-filtered through a 0.45-??m pore-size filter disc. The filter, with the thin film of precipitate, is supported between two sheets of Mylar?? film for analysis. Good agreement is shown between data reported in this study and literature values reported by epithermal neutron-activation analysis and spectrofluorimetry. The method can be made quantitative by utilizing a secondary precipitation to assure complete recovery of the Se. The X-ray method offers fast turn-around time and a reasonably high production rate. ?? 1981.

  1. In situ observation of dynamic electrodeposition processes by soft x-ray fluorescence microspectroscopy and keyhole coherent diffractive imaging

    Science.gov (United States)

    Bozzini, Benedetto; Kourousias, George; Gianoncelli, Alessandra

    2017-03-01

    This paper describes two novel in situ microspectroscopic approaches to the dynamic study of electrodeposition processes: x-ray fluorescence (XRF) mapping with submicrometric space resolution and keyhole coherent diffractive imaging (kCDI) with nanometric lateral resolution. As a case study, we consider the pulse-plating of nanocomposites with polypyrrole matrix and Mn x Co y O z dispersoids, a prospective cathode material for zinc-air batteries. This study is centred on the detailed measurement of the elemental distributions developing in two representative subsequent growth steps, based on the combination of in situ identical-location XRF microspectroscopy—accompanied by soft-x ray absorption microscopy—and kCDI. XRF discloses space and time distributions of the two electrodeposited metals and kCDI on the one hand allows nanometric resolution and on the other hand provides complementary absorption as well as phase contrast modes. The joint information derived from these two microspectroscopies allows measurement of otherwise inaccessible observables that are a prerequisite for electrodeposition modelling and control accounting for dynamic localization processes.

  2. Pure hydroxyapatite phantoms for the calibration of in vivo X-ray fluorescence systems of bone lead and strontium quantification.

    Science.gov (United States)

    Da Silva, Eric; Kirkham, Brian; Heyd, Darrick V; Pejović-Milić, Ana

    2013-10-01

    Plaster of Paris [poP, CaSO4·(1)/(2) H2O] is the standard phantom material used for the calibration of in vivo X-ray fluorescence (IVXRF)-based systems of bone metal quantification (i.e bone strontium and lead). Calibration of IVXRF systems of bone metal quantification employs the use of a coherent normalization procedure which requires the application of a coherent correction factor (CCF) to the data, calculated as the ratio of the relativistic form factors of the phantom material and bone mineral. Various issues have been raised as to the suitability of poP for the calibration of IVXRF systems of bone metal quantification which include its chemical purity and its chemical difference from bone mineral (a calcium phosphate). This work describes the preparation of a chemically pure hydroxyapatite phantom material, of known composition and stoichiometry, proposed for the purpose of calibrating IVXRF systems of bone strontium and lead quantification as a replacement for poP. The issue with contamination by the analyte was resolved by preparing pure Ca(OH)2 by hydroxide precipitation, which was found to bring strontium and lead levels to crystal structure of the material was found to be similar to that of the bone mineral component of NIST SRM 1486 (bone meal), as determined by powder X-ray diffraction spectrometry.

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

    Science.gov (United States)

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

    2011-01-01

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

  4. Quantification of manganese and mercury in toenail in vivo using portable X-ray fluorescence (XRF).

    Science.gov (United States)

    Zhang, Xinxin; Specht, Aaron J; Weisskopf, Marc G; Weuve, Jennifer; Nie, Linda H

    2018-03-01

    Toenail is an advantageous biomarker to assess exposure to metals such as manganese and mercury. Toenail Mn and Hg are in general analyzed by chemical methods such as inductively coupled plasma mass spectrometry and atomic absorption spectrophotometry. In this project, a practical and convenient technology-portable X-ray florescence (XRF)-is studied for the noninvasive in vivo quantification of manganese and mercury in toenail. The portable XRF method has advantages in that it does not require toenail clipping and it can be done in 3 min, which will greatly benefit human studies involving the assessment of manganese and mercury exposures. This study mainly focused on the methodology development and validation which includes spectral analysis, system calibration, the effect of toenail thickness, and the detection limit of the system. Manganese- and mercury-doped toenail phantoms were made. Calibration lines were established for these measurements. The results show that the detection limit for manganese is 3.65 μg/g (ppm) and for mercury is 0.55 μg/g (ppm) using 1 mm thick nail phantoms with 10 mm soft tissue underneath. We conclude that portable XRF is a valuable and sensitive technology to quantify toenail manganese and mercury in vivo.

  5. Green copper pigments biodegradation in cultural heritage: from malachite to moolooite, thermodynamic modeling, X-ray fluorescence, and Raman evidence.

    Science.gov (United States)

    Castro, Kepa; Sarmiento, Alfredo; Martínez-Arkarazo, Irantzu; Madariaga, Juan Manuel; Fernández, Luis Angel

    2008-06-01

    Moolooite (copper oxalate), a very rare compound, was found as a degradation product from the decay of malachite in several specimens of Cultural Heritage studied. Computer simulations, based on heterogeneous chemical equilibria, support the transformation of malachite to moolooite through the intermediate copper basic sulfates or copper basic chlorides, depending on the presence of available free sulfate or chloride anions in the chemical system. Raman and X-ray fluorescence spectral evidence found during the analysis of the three case studies investigated supported the model predictions. According to the study, the presence of lichens and other microorganisms might be responsible for the decay phenomena. This work tries to highlight the importance of biological attack on specimens belonging to Cultural Heritage and to demonstrate the consequences of oxalic acid, excreted by some of these microorganisms, on the conservation and preservation of artwork.

  6. Seasonal variation in trace and minor elements in Brazilian honey by total reflection X-ray fluorescence.

    Science.gov (United States)

    de Oliveira Resende Ribeiro, Roberta; Mársico, Eliane Teixeira; da Silva Carneiro, Carla; Simoes, Julia Siqueira; da Silva Ferreira, Micheli; de Jesus, Edgar Francisco Oliveira; Almeida, Eduardo; Junior, Carlos Adam Conte

    2015-03-01

    Honey is used as an alternative medicine and is a constituent of a healthy diet worldwide. Its composition is associated with botanical origin and, to some extent, geographical origin because soil and climate characteristics determine the melliferous flora. Also, the elements content in honey samples could give an indication of environmental pollution or geographical origin. The main purpose of this study was to evaluate seasonal patterns of essential elements of Brazilian honey. Honey was collected during spring, summer, autumn, and winter for 2 years to quantify K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Se, Br, and Sr using total reflection X-ray fluorescence spectroscopy (TXRF). Our results indicate no seasonal differences in concentration of Cr, Ni, Se, and Ti, although there were significant seasonal patterns in the composition of essential elements in honey, with higher concentrations of minor and trace elements, especially K and Ca of samples collected in spring and summer.

  7. Implementation of X-ray fluorescence microscopy for investigation of elemental abnormalities in central nervous system tissue

    Energy Technology Data Exchange (ETDEWEB)

    Chwiej, J. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland)]. E-mail: jchwiej@novell.ftj.agh.edu.pl; Szczerbowska-Boruchowska, M. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Wojcik, S. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Lankosz, M. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Chlebda, M. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Adamek, D. [Institute of Neurology, Collegium Medicum, Jagiellonian University, ul. Botaniczna-3, 31-503 Cracow (Poland); Tomik, B. [Institute of Neurology, Collegium Medicum, Jagiellonian University, ul. Botaniczna-3, 31-503 Cracow (Poland); Setkowicz, Z. [Department of Neuroanatomy, Institute of Zoology, Jagiellonian University, ul. Ingardena 6, 30-060 Cracow (Poland); Falkenberg, G. [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, Hamburg (Germany); Stegowski, Z. [Faculty of Physics and Applied Computer Science, AGH, University of Science and Technology, Al. Mickiewicza 30, 30-059 Cracow (Poland); Szczudlik, A. [Institute of Neurology, Collegium Medicum, Jagiellonian University, ul. Botaniczna-3, 31-503 Cracow (Poland)

    2005-09-29

    The microbeam synchrotron radiation X-ray fluorescence technique (micro-SRXRF) was applied to topographic and quantitative elemental analysis of human spinal cord tissue sections. The feasibility of this technique for the determination of elemental abnormalities caused by neurodegenerative disorder, i.e. amyotrophic lateral sclerosis (ALS), was verified. The applied measurement conditions allowed detecting: P, S, Cl, K, Ca, Fe, Cu, Zn and Br in thin tissue slices. Two-dimensional maps of the elemental distribution were recorded. Quantitative differences in elemental concentration between gray matter, nerve cells and white matter were observed for all analyzed cases. For the motor neuron bodies higher accumulation of S, Cl, K, Fe, Zn and Br was noticed. The results showed significant differences of elemental accumulation between the analyzed ALS cases. Moreover, the feasibility of using tissue sections fixed and embedded in paraffin for micro-SRXRF analysis was tested. These studies were performed on the samples of rat brain.

  8. Mapping the subcellular localization of Fe3O4@TiO2 nanoparticles by X-ray Fluorescence Microscopy

    Science.gov (United States)

    Yuan, Y.; Chen, S.; Gleber, S. C.; Lai, B.; Brister, K.; Flachenecker, C.; Wanzer, B.; Paunesku, T.; Vogt, S.; Woloschak, G. E.

    2013-10-01

    The targeted delivery of Fe3O4@TiO2 nanoparticles to cancer cells is an important step in their development as nanomedicines. We have synthesized nanoparticles that can bind the Epidermal Growth Factor Receptor, a cell surface protein that is overexpressed in many epithelial type cancers. In order to study the subcellular distribution of these nanoparticles, we have utilized the sub-micron resolution of X-ray Fluorescence Microscopy to map the location of Fe3O4@TiO2 NPs and other trace metal elements within HeLa cervical cancer cells. Here we demonstrate how the higher resolution of the newly installed Bionanoprobe at the Advanced Photon Source at Argonne National Laboratory can greatly improve our ability to distinguish intracellular nanoparticles and their spatial relationship with subcellular compartments.

  9. Determination of arsenic in geological materials by x-ray fluorescence spectrometry after solvent extraction and deposition on a filter

    Science.gov (United States)

    Hubert, A.E.

    1983-01-01

    Rock, soil, or sediment samples are decomposed with a mixture of nitric and sulphuric adds. After reduction from arsenic(V) with ammonium thiosulphate, arsenic(III) is extracted as the chlorocomplex into benzene from a sulphuric-hydrochloric acid medium. The benzene solution is transferred onto a filter-paper disc impregnated with a solution of sodium bicarbonate and potassium sodium tartrate, and the benzene allowed to evaporate. The arsenic present is determined by X-ray fluorescence. In a 0.5-g sample, 1-1000 ppm of arsenic can be determined. The close proximity of the lead L?? peak (2?? 48.73??), to the arsenic K?? peak (2?? 48.83??) does not cause any interference, because lead is not extracted under the experimental conditions. Arsenic values obtained are in agreement with those reported for various reference samples. ?? 1983.

  10. Development of a Silicon Drift Detector Array: An X-Ray Fluorescence Spectrometer for Remote Surface Mapping

    Science.gov (United States)

    Gaskin, Jessica A.; Carini, Gabriella A.; Wei, Chen; Elsner, Ronald F.; Kramer, Georgiana; De Geronimo, Gianluigi; Keister, Jeffrey W.; Zheng, Li; Ramsey, Brian D.; Rehak, Pavel; hide

    2009-01-01

    Over the past three years NASA Marshall Space Flight Center has been collaborating with Brookhaven National Laboratory to develop a modular Silicon Drift Detector (SDD) X-Ray Spectrometer (XRS) intended for fine surface mapping of the light elements of the moon. The value of fluorescence spectrometry for surface element mapping is underlined by the fact that the technique has recently been employed by three lunar orbiter missions; Kaguya, Chandrayaan-1, and Chang e. The SDD-XRS instrument we have been developing can operate at a low energy threshold (i.e. is capable of detecting Carbon), comparable energy resolution to Kaguya (<150 eV at 5.9 keV) and an order of magnitude lower power requirement, making much higher sensitivities possible. Furthermore, the intrinsic radiation resistance of the SDD makes it useful even in radiation-harsh environments such as that of Jupiter and its surrounding moons.

  11. Multielemental analysis in organic products and seed of linum by X-ray total reflection fluorescence with synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Serpa, Renata F.B.; Jesus, Edgar F.O. de; Lopes, Ricardo T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Lab. de Instrumentacao Nuclear]. E-mail: renata@lin.ufrj.br; Carmo, Maria da Graca T. do [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Nutricao; Moreira, Silvana [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil]. E-mail: silvana@fec.com.br

    2005-07-01

    The main goal of this study is to determining the trace and major elements levels in organic seeds samples, like soy, rice, bean and in Brazilian and Canadian linum seed by X-ray Total Reflection Fluorescence with Synchrotron Radiation (SR-TXRF). The measurements were carried out in the XRF beamline at the Light Synchrotron National Laboratory (Campinas, Brazil). The organic soy presented major concentrations of P, Ca, Ti, Fe, Ni, Cu, Zn, Br, Rb and Sr than organic bean and rice. Brazilian linum samples presented higher concentrations of S, P, Ca, Ni, Cu, Sr, Zr and Mo than Canadian one, even than organic samples. However potassium, iron and zinc were more pronounced in the Canadian seed of linum (author)

  12. X-Ray Fluorescence to Estimate the Maximum Temperature Reached at Soil Surface during Experimental Slash-and-Burn Fires.

    Science.gov (United States)

    Melquiades, Fábio L; Thomaz, Edivaldo L

    2016-05-01

    An important aspect for the evaluation of fire effects in slash-and-burn agricultural system, as well as in wildfire, is the soil burn severity. The objective of this study is to estimate the maximum temperature reached in real soil burn events using energy dispersive X-ray fluorescence (EDXRF) as an analytical tool, combined with partial least square (PLS) regression. Muffle-heated soil samples were used for PLS regression model calibration and two real slash-and-burn soils were tested as external samples in the model. It was possible to associate EDXRF spectra alterations to the maximum temperature reached in the heat affected soils with about 17% relative standard deviation. The results are promising since the analysis is fast, nondestructive, and conducted after the burn event, although local calibration for each type of burned soil is necessary. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  13. Raman microscopy and x-ray fluorescence analysis of pigments on medieval and Renaissance Italian manuscript cuttings.

    Science.gov (United States)

    Burgio, Lucia; Clark, Robin J H; Hark, Richard R

    2010-03-30

    Italian medieval and Renaissance manuscript cuttings and miniatures from the Victoria and Albert Museum were analyzed by Raman microscopy to compile a database of pigments used in different periods and different Italian regions. The palette identified in most manuscripts and cuttings was found to include lead white, gypsum, azurite, lazurite, indigo, malachite, vermilion, red lead, lead tin yellow (I), goethite, carbon, and iron gall ink. A few of the miniatures, such as the historiated capital "M" painted by Gerolamo da Cremona and the Petrarca manuscript by Bartolomeo Sanvito, are of exceptional quality and were analyzed extensively; some contained unusual materials. The widespread usage of iron oxides such as goethite and hematite as minor components of mixtures with azurite is particularly notable. The use of a needle-shaped form of iron gall ink as a pigment rather than a writing material was established by both Raman microscopy and x-ray fluorescence spectroscopy for the Madonna and Child by Franco de' Russi.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  15. Individual particle analysis of coarse air suspended particulate material by synchrotron radiation X-ray micro fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Melo Junior, Ariston [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Perez, Carlos Alberto [Laboratorio Nacional de Luz Sincrotron (LNLS), Campinas, SP (Brazil)]. E-mail: perez@lnls.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br

    2005-07-01

    The purpose of this work is evaluate the size of individual particles present in the air suspended particulate material collected in Campinas, Sao Paulo State, and analyze quantitatively the particles using the synchrotron radiation X-ray micro fluorescence ({mu}-SRXRF) associated with the fundamental parameter method to correct attenuation/absorption effects by the matrix. The particles analyzed have size between 50-10 {mu}m and to perform the spatial distribution a white beam of synchrotron radiation condensed by a conical capillary (13 {mu}m diameter) was used. For the quantitative analysis punctual measures in thin films standards in Mylar subtract were performed. The elements detected were Si, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb. (author)

  16. X-ray fluorescence and imaging analyses of paintings by the Brazilian artist Oscar Pereira Da Silva

    Science.gov (United States)

    Campos, P. H. O. V.; Kajiya, E. A. M.; Rizzutto, M. A.; Neiva, A. C.; Pinto, H. P. F.; Almeida, P. A. D.

    2014-02-01

    Non-destructive analyses, such as EDXRF (Energy-Dispersive X-Ray Fluorescence) spectroscopy, and imaging were used to characterize easel paintings. The analyzed objects are from the collection of the Pinacoteca do Estado de São Paulo. EDXRF results allowed us to identify the chemical elements present in the pigments, showing the use of many Fe-based pigments, modern pigments, such as cobalt blue and cadmium yellow, as well as white pigments containing lead and zinc used by the artist in different layers. Imaging analysis was useful to identify the state of conservation, the localization of old and new restorations and also to detect and unveil the underlying drawings revealing the artist's creative processes.

  17. Synchrotron x-ray fluorescence analyses of stratospheric cosmic dust: New results for chondritic and nickel-depleted particles

    Energy Technology Data Exchange (ETDEWEB)

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

    1989-06-01

    Trace element abundance determinations were performed using synchrotron x-ray fluorescence on nine particles collected from the stratosphere and classified as ''cosmic''. Improvements to the Synchrotron Light Source allowed the detection of all elements between Cr and Mo, with the exceptions of Co and As, in our largest particle. The minor and trace element abundance patterns of three Ni-depleted particles were remarkably similar to those of extraterrestrial igneous rocks. Fe/Ni and Fe/Mn ratios suggest that one of these may be of lunar origin. All nine particles exhibited an enrichment in Br, ranging form 1.3 to 38 times the Cl concentration. Br concentrations were uncorrelated with particle size, as would be expected for a surface correlated component acquires from the stratosphere. 27 refs., 4 figs., 2 tabs.

  18. Probing Intracellular Element Concentration Changes during Neutrophil Extracellular Trap Formation Using Synchrotron Radiation Based X-Ray Fluorescence.

    Directory of Open Access Journals (Sweden)

    Björn De Samber

    Full Text Available High pressure frozen (HPF, cryo-substituted microtome sections of 2 μm thickness containing human neutrophils (white blood cells were analyzed using synchrotron radiation based X-ray fluorescence (SR nano-XRF at a spatial resolution of 50 nm. Besides neutrophils from a control culture, we also analyzed neutrophils stimulated for 1-2 h with phorbol myristate acetate (PMA, a substance inducing the formation of so-called Neutrophil Extracellular Traps (or NETs, a defense system again pathogens possibly involving proteins with metal chelating properties. In order to gain insight in metal transport during this process, precise local evaluation of elemental content was performed reaching limits of detection (LODs of 1 ppb. Mean weight fractions within entire neutrophils, their nuclei and cytoplasms were determined for the three main elements P, S and Cl, but also for the 12 following trace elements: K, Ca, Mn, Fe, Co, Ni, Cu, Zn, Se, Br, Sr and Pb. Statistical analysis, including linear regression provided objective analysis and a measure for concentration changes. The nearly linear Ca and Cl concentration changes in neutrophils could be explained by already known phenomena such as the induction of Ca channels and the uptake of Cl under activation of NET forming neutrophils. Linear concentration changes were also found for P, S, K, Mn, Fe, Co and Se. The observed linear concentration increase for Mn could be related to scavenging of this metal from the pathogen by means of the neutrophil protein calprotectin, whereas the concentration increase of Se may be related to its antioxidant function protecting neutrophils from the reactive oxygen species they produce against pathogens. We emphasize synchrotron radiation based nanoscopic X-ray fluorescence as an enabling analytical technique to study changing (trace element concentrations throughout cellular processes, provided accurate sample preparation and data-analysis.

  19. Factors influencing bone lead concentration in a suburban community assessed by noninvasive K x-ray fluorescence.

    Science.gov (United States)

    Kosnett, M J; Becker, C E; Osterloh, J D; Kelly, T J; Pasta, D J

    1994-01-19

    To determine the influence of demographic, exposure and medical factors on the bone lead concentration of subjects with background (nonindustrial) environmental lead exposure. Survey. Suburban residential community. A total of 101 subjects (49 males, 52 females; aged 11 to 78 years) were recruited from 49 of 123 households geographically located in a suburban residential neighborhood unexposed to any major source of industrial lead emissions. Cortical bone lead concentrations in the midshaft of the tibia were noninvasively measured by in vivo K x-ray fluorescence. Blood lead concentrations were measured by anodic stripping voltammetry. An administered questionnaire assessed potential sources of lead exposure and medical conditions affecting bone metabolism. After the exclusion of one outlier, log-transformed bone lead concentration was highly correlated with age (r = .71; P < or = .0001). Bone lead concentration showed no significant change up to age 20 years, increased with the same slope in men and women between ages 20 and 55 years, and then increased at a faster rate in men older than 55 years. In addition to the variables age and sex, the best fitting multiple regression model for bone lead concentration (R2 = .66; P < or = .0001) revealed a positive correlation with total pack-years of cigarette smoking and a negative correlation with a history of having nursed an infant for longer than 2 weeks. Blood lead concentrations of the subjects were low (geometric mean, 0.24 mumol/L [4.9 micrograms/dL]) and after log transformation were weakly correlated with log-transformed bone lead concentration (r = .23; P = .02). The age- and sex-related increases in bone lead concentration found by K x-ray fluorescence concur with published postmortem studies of bone lead concentration and are consistent with the kinetics of bone turnover and secular trends in lead exposure. These data help to establish a reference range for assessing the lead burden of other populations with

  20. Documenting mudstone heterogeneity by use of principal component analysis of X-ray diffraction and portable X-ray fluorescence data: A case study in the Triassic Shublik Formation, Alaska North Slope

    Science.gov (United States)

    Boehlke, Adam; Whidden, Katherine J.; Benzel, William M.

    2017-01-01

    Determining the chemical and mineralogical variability within fine-grained mudrocks poses analytical challenges but is potentially useful for documenting subtle stratigraphic differences in physicochemical environments that may influence petroleum reservoir properties and behavior. In this study, we investigate the utility of combining principal component analysis (PCA) of X-ray diffraction (XRD) data and portable X-ray fluorescence (pXRF) data to identify simplifying relationships within a large number of samples and subsequently evaluate a subset that encompasses the full spectrum or range of mineral and chemical variability within a vertical section. Samples were collected and analyzed from a vertical core of the Shublik Formation, a heterogeneous, phosphate-rich, calcareous mudstone-to-marl unit deposited in the Arctic Alaska Basin (AAB) during the Middle and Late Triassic. The Shublik is a major petroleum source rock in the Alaskan North Slope, and is considered a prime target for continuous self-sourced resource plays.

  1. X-ray fluorescence analysis of Pb, Fe and Zn in kohl

    Directory of Open Access Journals (Sweden)

    Eman Daar

    Full Text Available Kohl, a facial salve used in ancient times as a symbol of affluence, now enjoys more widespread traditional followings, for cosmetic, religious and supposed medicinal purposes. Popularly used by women and men of all ages, particularly those of North African, Middle Eastern, Southern Asia, Japanese and Chinese origins, it is also known to be used on neonates and children from such populations. With small-scale producers of kohl possessing a growing awareness of the adverse market impact of products that contain (lead Pb and other toxicity related elements, some claim their products to be Pb-free, offering an apparent change from the more traditional galena-based (lead sulphide media. Among the published physiological effects of exposure to Pb is that it replaces Ca in bones and teeth, making them weak and fragile, other impacts including nephrotoxicity, also linked with increased Pb blood levels in studies in Oman, Canada, Saudi Arabia, India and Pakistan. Current study involves XRF analysis of Pb, Fe and Zn concentrations in 135 samples of kohl from nine randomly selected suppliers (15 samples of each brand being represented. In pursuit of this, use was made of an in-house assembled facility comprising compact high-performance components, the arrangement offering sufficient sensitivity for the purposes of present study. In most of the samples investigated in the present study observation has been made of concentrations of Pb at elevated levels, quantification of those levels also demonstrating a need to address self-attenuation by the Pb itself. Significant concentration of Fe have also been found in several of the samples. Keywords: X-ray florescence, Pb, Fe and Zn contamination, Kohl

  2. Quantification of zinc-porphyrin in dry-cured ham products by spectroscopic methods Comparison of absorption, fluorescence and X-ray fluorescence spectroscopy.

    Science.gov (United States)

    Laursen, Kristoffer; Adamsen, Christina E; Laursen, Jens; Olsen, Karsten; Møller, Jens K S

    2008-03-01

    Zinc-protoporphyrin (Zn-pp), which has been identified as the major pigment in certain dry-cured meat products, was extracted with acetone/water (75%) and isolated from the following meat products: Parma ham, Iberian ham and dry-cured ham with added nitrite. The quantification of Zn-pp by electron absorption, fluorescence and X-ray fluorescence (XRF) spectroscopy was compared (concentration range used [Zn-pp]=0.8-9.7μM). All three hams were found to contain Zn-pp, and the results show no significant difference among the content of Zn-pp quantified by fluorescence, absorbance and X-ray fluorescence spectroscopy for Parma ham and Iberian ham. All three methods can be used for quantification of Zn-pp in acetone/water extracts of different ham types if the content is higher than 1.0ppm. For dry-cured ham with added nitrite, XRF was not applicable due to the low content of Zn-pp (ham extracts investigated (limit of detection; Fe⩽1.8ppm), it allows the conclusion that iron containing pigments, e.g., heme, do not contribute to the noticeable red colour observed in some of the extracts.

  3. In situ X-ray fluorescence-based method to differentiate among red ochre pigments and yellow ochre pigments thermally transformed to red pigments of wall paintings from Pompeii.

    Science.gov (United States)

    Marcaida, Iker; Maguregui, Maite; Fdez-Ortiz de Vallejuelo, Silvia; Morillas, Héctor; Prieto-Taboada, Nagore; Veneranda, Marco; Castro, Kepa; Madariaga, Juan Manuel

    2017-06-01

    Most of the magnificent wall paintings from the ancient city of Pompeii are decorated with red and yellow colors coming from the ochre pigments used. The thermal impact of the pyroclastic flow from the eruption of Vesuvius, in AD 79, promoted the transformation of some yellow painted areas to red. In this work, original red ochre, original yellow ochre, and transformed yellow ochre (nowadays showing a red color) of wall paintings from Pompeian houses (House of Marcus Lucretius and House of Gilded Cupids) were analyzed by means of a handheld energy-dispersive X-ray fluorescence spectrometer to develop a fast method that allows chemical differentiation of the original red ochre and the transformed yellow ochre. Principal component analysis of the multivariate obtained data showed that arsenic is the tracer element to distinguish between both red colored ochres. Moreover, Pompeian raw red and yellow ochre pigments recovered from the burial were analyzed in the laboratory with use of a benchtop energy-dispersive X-ray fluorescence spectrometer to confirm the elemental composition and the conclusions drawn from the in situ analysis according to the yellow ochre pigment transformation in real Pompeian wall paintings.

  4. Scanning Transmission Electron microscope Studies of Deep-Frozen Unfixed Muscle Correlated with Spatial Localization of Intracellular Elements by Fluorescent X-Ray Analysis

    Science.gov (United States)

    Bacaner, Marvin; Broadhurst, John; Hutchinson, Thomas; Lilley, John

    1973-01-01

    Thin sections of deep-frozen unfixed muscle were studied in a scanning electron microscope modified for transmission imaging and equipped with a “cryostage” for vacuum compatibility of hydrated tissue. With an energy-dispersive x-ray analysis system, intracellular atomic species in the scan beam path were identified by their fluorescent x-rays and spatially localized in correlation with the electron optical image of the microstructure. Marked differences are noted between the ultrastructure of deep-frozen hydrated muscle and that of fixed dehydrated muscle. In frozen muscle, myofibrils appear to be composed of previously undescribed longitudinal structures between 400-1000 Å wide (“macromyofilaments”). The usual myofilaments, mitochondria, and sarcoplasmic reticulum were not seen unless the tissue was “fixed” before examination. Fluorescent x-ray analysis of the spatial location of constituent elements clearly identified all elements heavier than Na. Intracellular Cl was relatively higher than expected. Images PMID:4587251

  5. Portable X-ray Fluorescence and Infrared Fluorescence Imaging Studies of Cadmium Yellow Alteration in Paintings by Edward Munch and Henri matisse in Oslo, Copenhagen, and San Francisco

    DEFF Research Database (Denmark)

    Mass, Jennifer; Uffelman, Erich; Buckley, Barbara

    2016-01-01

    The identification of altered cadmium yellow paints in early modernist works is critical to their stabilization and to the long-term preservation of the paintings in which they occur. The identification of incipient photoalteration of these pigments, before there is visual evidence...... of their chemical degradation, is of particular concern. The alteration of these pigments causes chalking, flaking, fading, and darkening of the yellow paints, leading to irreversible changes in the physical and chemical structure of the paint layer and dramatically altering the appearance of the work. Standoff......-induced visible fluorescence, ultraviolet-induced infrared fluorescence, multispectral imaging, and X-ray fluorescence. Questions addressed included the following: Is the imaging method being tested comprehensive? Is it efficient at surveying an entire painting? Does it reveal the state of preservation...

  6. Spatially resolved x-ray fluorescence spectroscopy of beryllium capsule implosions at the NIF

    Science.gov (United States)

    MacDonald, M. J.; Bishel, D. T.; Saunders, A. M.; Scott, H. A.; Kyrala, G.; Kline, J.; MacLaren, S.; Thorn, D. B.; Yi, S. A.; Zylstra, A. B.; Falcone, R. W.; Doeppner, T.

    2017-10-01

    Beryllium ablators used in indirectly driven inertial confinement fusion implosions are doped with copper to prevent preheat of the cryogenic hydrogen fuel. Here, we present analysis of spatially resolved copper K- α fluorescence spectra from the beryllium ablator layer. It has been shown that K- α fluorescence spectroscopy can be used to measure plasma conditions of partially ionized dopants in high energy density systems. In these experiments, K-shell vacancies in the copper dopant are created by the hotspot emission at stagnation, resulting in K-shell fluorescence at bang time. Spatially resolved copper K- α emission spectra are compared to atomic kinetics and radiation code simulations to infer density and temperature profiles. This work was supported by the US DOE under Grant No. DE-NA0001859, under the auspices of the US DOE by Lawrence Livermore National Laboratory under Contract No. DE-AC52-07NA27344, and by Los Alamos National Laboratory under contract DE-AC52-06NA52396.

  7. Multielement analysis of X-Ray fluorescence of Nerium oleander L. Leaves in metropolitan region of Rio de Janeiro

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Ramon S.; Sanches, Francis Anna C.R.A.; Neves, Arthur O.P.; Oliveira, Davi F.; Anjos, Marcelino J., E-mail: ramonziosp@yahoo.com.br, E-mail: francissanches@gmail.com, E-mail: arthur.nevess@yahoo.com.br, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Fisica. Departamento de Fisica Aplicada e Termodinamica

    2015-07-01

    Some plants are used in the detection of the air pollutants due to leaves ability to absorb the pollutants through their stomata and the cuticle, thus, the plants leaves work as a natural sample of the air emissions that are deposited in their self. However, the foliar analysis of these vegetal species can be used to environmental monitoring. The Nerium oleander L. is a specie of plant commonly used as an environmental biomonitor. In this study, Nerium oleander L. leaves were used as biomonitors to evaluate the levels of environmental pollutants in a sub-region in the Metropolitan Region of Rio de Janeiro-Brazil through Energy Dispersive X-ray Fluorescence technique - EDXRF. The EDXRF system was developed in the own laboratory and consist of a portable XRF system formed by a mini X-ray tube of low power (anode of Ag and operated in 15 kV/50 μA and 35 kV/50 μA) and a SiPIN detector. Samples of Nerium oleander L. were collected from adult plants drawn randomly so as not favoring one side of the plant. The samples were collected during the year seasons (summer and winter). It was detected the concentration of 13 elements: S, Cl, K, Ca, Mn, Fe, Cu, Zn, Br, Rb, Sr, Ba and Pb, and obtain elemental maps of the regions of study. The study shows that the use of EDXRF technique associated to the Nerium oleander L. leaves used as biomonitor is an efficient, precise, fast and low-cost option for air pollutants analysis. (author)

  8. Quantitative analysis of trace palladium contamination in solution using electrochemical X-ray fluorescence (EC-XRF).

    Science.gov (United States)

    Ayres, Zoë J; Newton, Mark E; Macpherson, Julie V

    2016-06-07

    The application of electrochemical X-ray fluorescence (EC-XRF), for the detection of palladium (Pd) contamination in a range of solutions containing electrochemically active compounds, present in excess and relevant to the pharmaceutical and food industries, is reported. In EC-XRF, EC is used to electrochemically pre-concentrate metal on an electrode under forced convection conditions, whilst XRF is employed to spectroscopically quantify the amount of metal deposited, which quantitatively correlates with the original metal concentration in solution. Boron doped diamond is used as the electrode due to its very wide cathodic window and the fact that B and C are non-interfering elements for XRF analysis. The effect of several parameters on the Pd XRF signal intensity are explored including: deposition potential (Edep), deposition time (tdep) and Pd(2+) concentration, [Pd(2+)]. Under high deposition potentials (Edep = -1.5 V), the Pd XRF peak intensity varies linearly with both tdep and [Pd(2+)]. Quantification of [Pd(2+)] is demonstrated in the presence of excess acetaminophen (ACM), l-ascorbic acid, caffeine and riboflavin. We show the same Pd XRF signal intensity (for [Pd(2+)] = 1.1 μM and tdep = 325 s) is observed, i.e. same amount of Pd is deposited on the electrode surface, irrespective of whether these redox active molecules are present or absent. For tdep = 900 s we report a limit of detection for [Pd(2+)] of 3.6 ppb (34 nM). Even lower LODs are possible by increasing tdep or by optimising the X-ray source specifically for Pd. The work presented for Pd detection in the presence of ACM, achieves the required detection sensitivity stipulated by international pharmacopeia guidelines.

  9. Copper Uptake, Intracellular Localization, and Speciation in Marine Microalgae Measured by Synchrotron Radiation X-ray Fluorescence and Absorption Microspectroscopy.

    Science.gov (United States)

    Adams, Merrin S; Dillon, Carolyn T; Vogt, Stefan; Lai, Barry; Stauber, Jennifer; Jolley, Dianne F

    2016-08-16

    Metal toxicity to aquatic organisms depends on the speciation of the metal and its binding to the critical receptor site(s) (biotic ligand) of the organism. The intracellular nature of the biotic ligand for Cu in microalgal cells was investigated using the high elemental sensitivity of microprobe synchrotron radiation X-ray fluorescence (SR-XRF) and X-ray absorption near-edge spectroscopy (XANES). The marine microalgae, Ceratoneis closterium, Phaeodactylum tricornutum, and Tetraselmis sp. were selected based on their varying sensitivities to Cu (72-h 50% population growth inhibitions of 8-47 μg Cu/L). Intracellular Cu in control cells was similar for all three species (2.5-3.2 × 10(-15) g Cu/cell) and increased 4-fold in C. closterium and Tetraselmis sp. when exposed to copper, but was unchanged in P. tricornutum (72-h exposure to 19, 40, and 40 μg Cu/L, respectively). Whole cell microprobe SR-XRF identified endogenous Cu in the central compartment (cytoplasm) of control (unexposed) cells. After Cu exposure, Cu was colocated with organelles/granules dense in P, S, Ca, and Si and this was clearly evident in thin sections of Tetraselmis sp. XANES indicated coexistence of Cu(I) and Cu(II) in control and Cu-exposed cells, with the Cu ligand (e.g., phytochelatin) in P. tricornutum different from that in C. closterium and Tetraselmis sp. This study supports the hypothesis that Cu(II) is reduced to Cu(I) and that polyphosphate bodies and phytochelatins play a significant role in the internalization and detoxification of Cu in marine microalgae.

  10. Elemental analysis of multilayer samples by means of combined laser ablation and x-ray fluorescence spectrometry

    Science.gov (United States)

    Fiorini, C.; Gianoncelli, A.; Longoni, A.; Comelli, D.; D'Andrea, C.; Valentini, G.

    2003-02-01

    Even though absolutely noninvasive techniques are ideally required for the analysis of valuable works of art, in some cases, the historical study or the restoration would benefit from deep investigations that require some kind of alterations on the sample. This is the case when a stratigraphic analysis of a paint has to be carried out to determine pigments and ligants used by the painter. To perform this task, a fully automated device working in situ without physical contact with the sample is certainly the best choice in terms of minimal damage, ease of operation, and quickness of analysis. Such a device could result from the combination of the state of the art portable x-ray fluorescence (XRF) analyzer with a digging tool capable of micrometric control of positioning and depth of operation. In this article, we propose a new method for the determination of chemical element distribution in multilayer samples, based on the use of an alternate sequence of laser photoablations and XRF analysis. The laser source used in this work is a flash lamp pumped Er:YAG laser (2.94 μm), assembled in our laboratories. It operates at a repetition rate of 8 Hz in a Q-switching regime and generates an average power of 60 mW. The XRF spectrometer is a portable instrument based on a Peltier-cooled silicon drift detector (operated at about -10 °C) which is characterized by an energy resolution of about 155 eV full width at half maximum at 6 keV. An x-ray tube with a tungsten anode is used as excitation source. In this article, the measurement technique is described and the first experimental results obtained on samples composed by layers of different thickness and composition are presented.

  11. Elemental analysis of human amniotic fluid and placenta by total-reflection X-ray fluorescence and energy-dispersive X-ray fluorescence: child weight and maternal age dependence

    Science.gov (United States)

    Carvalho, M. L.; Custódio, P. J.; Reus, U.; Prange, A.

    2001-11-01

    This work is an attempt to evaluate the possible influence of the mother's age in trace element concentrations in human amniotic fluid and placenta and whether these concentrations are correlated to the weight of the newborn infants. Total-reflection X-ray fluorescence (TXRF) was used to analyze 16 amniotic fluid samples, and the placenta samples were analyzed by energy dispersive X-ray fluorescence (EDXRF). The whole samples were collected during delivery from healthy mothers and healthy infants and full-term pregnancies. According to the age of the mother, three different groups were considered: 20-25, 25-30 and 30-40 years old. Only two mothers were aged more than 35 years. The weight of the infants ranged from 2.56 to 4.05 kg and three groups were also considered: 2.5-3, 3-3.5 and 3.5-4 kg. The organic matrix of the amniotic fluid samples was removed by treatment with HNO 3 followed by oxygen plasma ashing. Yttrium was used as the internal standard for TXRF analysis. Placenta samples were lyophilized and analyzed by EDXRF without any chemical treatment. Very low levels of Ni and Sr were found in the amniotic fluid samples, and were independent of the age of the mother and weight of the child. Cr, Mn, Se and Pb were at the level of the detection limit. Zn, considered one of the key elements in neonatal health, was not significantly different in the samples analyzed; however, it was weakly related to birth weigh. The concentrations obtained ranged from 0.11 to 0.92 mg/l and 30 to 65 μg/g in amniotic fluid and placenta, respectively. The only two elements which seemed to be significantly correlated with mother's age and newborn weight were Ca and Fe for both types of sample: Ca levels were increased in heavier children and older mothers; however, Fe increased with increasing maternal age, but decreased for heavier babies. The same conclusions were obtained for placenta and amniotic fluid samples. Cu is closely associated with Fe in its function in the organism

  12. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence.

    Science.gov (United States)

    Wobrauschek, P; Prost, J; Ingerle, D; Kregsamer, P; Misra, N L; Streli, C

    2015-08-01

    The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm(2) active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.

  13. A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence

    Energy Technology Data Exchange (ETDEWEB)

    Wobrauschek, P., E-mail: wobi@ati.ac.at; Prost, J.; Ingerle, D.; Kregsamer, P.; Streli, C. [Atominstitut, TU Wien, Stadionallee 2, 1020 Vienna (Austria); Misra, N. L. [Fuel Chemistry Division, Bhabha Atomic Research Centre (BARC), Mumbai 400085 (India)

    2015-08-15

    The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm{sup 2} active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.

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

    Science.gov (United States)

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

    2015-11-01

    Microprobe X-ray fluorescence tomography was used to investigate metal poison deposition in individual, intact and industrially deactivated fluid catalytic cracking (FCC) particles at two differing catalytic life-stages. 3 D multi-element imaging, at submicron resolution was achieved by using a large-array Maia fluorescence detector. Our results show that Fe, Ni and Ca have significant concentration at the exterior of the FCC catalyst particle and are highly co-localized. As concentrations increase as a function of catalytic life-stage, the deposition profiles of Fe, Ni, and Ca do not change significantly. V has been shown to penetrate deeper into the particle with increasing catalytic age. Although it has been previously suggested that V is responsible for damaging the zeolite components of FCC particles, no spatial correlation was found for V and La, which was used as a marker for the embedded zeolite domains. This suggests that although V is known to be detrimental to zeolites in FCC particles, a preferential interaction does not exist between the two.

  15. Quantification of single fluid inclusions by combining synchrotron radiation-induced micro-X-ray fluorescence and transmission.

    Science.gov (United States)

    Cauzid, J; Philippot, P; Somogyi, A; Simionovici, A; Bleuet, P

    2004-07-15

    Fluid inclusions represent the only direct samples of ancient fluids in many crustal rocks; precise knowledge of their chemical composition provides crucial information to model paleofluid-rock interactions and hydrothermal transport processes. Owing to its nondestructive character, micrometer-scale spatial resolution, and high sensitivity, synchrotron radiation-induced micro-X-ray fluorescence has received great interest for the in situ multielement analysis of individual fluid inclusions. Major uncertainties associated with the quantitative analysis of single fluid inclusions arise from the inclusion depth and the volume of fluid sampled by the incident beam. While the depth can be extracted directly from the fluorescence spectrum, its volume remains a major source of uncertainty. The present study performed on natural and synthetic inclusions shows that the inclusion thickness can be accurately evaluated from transmission line scans. Experimental data matched numerical simulations based on an elliptical inclusion geometry. However, for one nonelliptical inclusion, the experimental data were confirmed using a computed absorption tomography reconstruction. Good agreement between the imaging and scanning techniques implies that the latter provides reliable fluid thickness values independent of the shape of the inclusion. Taking into consideration the incident angle, the incident beam energy, the inclusion fluid salinity, and the transmission measurement stability resulted in errors of 0.3-2 microm on calculated fluid inclusion thicknesses.

  16. L X-ray fluorescence cross sections experimentally determined for elements with 45

    Energy Technology Data Exchange (ETDEWEB)

    Bonzi, Edgardo V., E-mail: bonzie@famaf.unc.edu.ar [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, Ciudad Universitaria-5010, Cordoba (Argentina); Badiger, Nagappa M. [Departments of Physics, Karnatak University, Dharwad 580 003, Karnataka (India); Grad, Gabriela B. [Facultad de Matematica, Astronomia y Fisica, Universidad Nacional de Cordoba, Ciudad Universitaria-5010, Cordoba (Argentina); Barrea, Raul A. [The Biophysics Collaborative Access Team (BioCAT), Dept of Biological Chemical, and Physical Sciences, Illinois Institute of Technology, Chicago, IL 60616 (United States); Figueroa, Rodolo G. [Departamento de Cs. Fisicas, Universidad de La Frontera, Temuco (Chile)

    2012-04-15

    Experimental determination of L fluorescence cross-sections for elements with 45X-ray photons, Ll, L{alpha}, L{beta}{sub I}, L{beta}{sub II}, L{gamma}{sub {Iota}} and L{gamma}{sub {Iota}{Iota}} produced in the target were measured using a Si(Li) detector. The experimental set-up provided a low background by using linearly polarized monoenergetic photon beam, improving the signal-to-noise ratio. The experimental cross sections obtained in this work were compared with data calculated using coefficients from , , and Scofield and Puri et al. (1993, 1995) - Highlights: Black-Right-Pointing-Pointer Experimental data of L fluorescence cross-sections with 45

  17. FMT-XCT: in vivo animal studies with hybrid fluorescence molecular tomography-X-ray computed tomography.

    Science.gov (United States)

    Ale, Angelique; Ermolayev, Vladimir; Herzog, Eva; Cohrs, Christian; de Angelis, Martin Hrabé; Ntziachristos, Vasilis

    2012-06-01

    The development of hybrid optical tomography methods to improve imaging performance has been suggested over a decade ago and has been experimentally demonstrated in animals and humans. Here we examined in vivo performance of a camera-based hybrid fluorescence molecular tomography (FMT) system for 360° imaging combined with X-ray computed tomography (XCT). Offering an accurately co-registered, information-rich hybrid data set, FMT-XCT has new imaging possibilities compared to stand-alone FMT and XCT. We applied FMT-XCT to a subcutaneous 4T1 tumor mouse model, an Aga2 osteogenesis imperfecta model and a Kras lung cancer mouse model, using XCT information during FMT inversion. We validated in vivo imaging results against post-mortem planar fluorescence images of cryoslices and histology data. Besides offering concurrent anatomical and functional information, FMT-XCT resulted in the most accurate FMT performance to date. These findings indicate that addition of FMT optics into the XCT gantry may be a potent upgrade for small-animal XCT systems.

  18. Determination of Mn, Fe, Ni, Cu, Zn and Pb contents in samples of apple trees by radionuclide X-ray fluorescence analysis

    Energy Technology Data Exchange (ETDEWEB)

    Bumbalova, A.; Havranek, E.; Harangozo, M. (Komenskeho Univ., Bratislava (Czechoslovakia). Farmaceuticka Fakulta)

    1982-12-01

    The applicability of the radionuclide X-ray fluorescence analysis (RXFA) for qualitative and quantitative evaluation of environmental plant samples is discussed and examples of determination of Mn, Fe, Ni, Cu, Zn, Pb in samples of apple trees are given. The instrumentation, the standard and sample preparation are also presented.

  19. LABORATORY EVALUATION OF SIX NEW/MODIFIED PORTABLE X-RAY FLUORESCENCE SPECTROMETERS FOR THE MEASUREMENT OF LEAD IN CHARACTERIZED PAINT FILMS AND RESEARCH MATERIAL BOARDS (APPENDICES)

    Science.gov (United States)

    A laboratory study was performed in 1994-1995 to identify and estimate the influence of key characteristics for evaluating the performance of portable X-ray fluorescence (XRF) spectrometers. Six new/modified spectrometers, including HNU SEFA-Pb, Metorex X-MET, Niton X-L, Radiat...

  20. LABORATORY EVALUATION OF SIX NEW/MODIFIED PORTABLE X-RAY FLUORESCENCE SPECTROMETERS FOR THE MEASUREMENT OF LEAD IN CHARACTERIZED PAINT FILMS AND RESEARCH MATERIAL BOARDS (TECHNICAL REPORT)

    Science.gov (United States)

    A laboratory study was performed in 1994-1995 to identify and estimate the influence of key characteristics for evaluating the performance of portable X-ray fluorescence (XRF) spectrometers. Six new/modified spectrometers, including HNU SEFA-Pb, Metorex X-MET, Niton X-L, Radiat...

  1. Synchrotron-based X-ray Fluorescence Microscopy in Conjunction with Nanoindentation to Study Molecular-Scale Interactions of Phenol–Formaldehyde in Wood Cell Walls

    Science.gov (United States)

    Joseph E. Jakes; Christopher G. Hunt; Daniel J. Yelle; Linda Lorenz; Kolby Hirth; Sophie-Charlotte Gleber; Stefan Vogt; Warren Grigsby; Charles R. Frihart

    2015-01-01

    Understanding and controlling molecular-scale interactions between adhesives and wood polymers are critical to accelerate the development of improved adhesives for advanced wood-based materials. The submicrometer resolution of synchrotron-based X-ray fluorescence microscopy (XFM) was found capable of mapping and quantifying infiltration of Br-labeled phenol−...

  2. The determination of major and some minor constituents in lead zirconate-titanate compositions by x-ray fluorescence and atomic absorption spectrometry

    NARCIS (Netherlands)

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

    1972-01-01

    An accurate X-ray fluorescence spectrometric method is described for the determination of lead, zirconium and titanium in lead zirconate-titanate ceramics. Careful matching of samples and standards by a borax fusion method resulted in a relative standard deviation of about 0.2% for the major

  3. X-ray fluorescence core scanning of wet marine sediments: methods to improve quality and reproducibility of high-resolution paleoenvironmental records

    NARCIS (Netherlands)

    Hennekam, R.; de Lange, G.

    2012-01-01

    X-ray fluorescence (XRF) core-scanning is a convenient non-destructive tool to rapidly assess elemental variations in unprocessed sediments. However, substantial analytical deviations may occur in such data due to physical sedimentary properties. The consequences of these artifacts on element

  4. Applicability of X-ray fluorescence spectroscopy as method to determine thickness and composition of stacks of metal thin films: A comparison with imaging and profilometry

    NARCIS (Netherlands)

    Vrielink, J.A.M.; Tiggelaar, Roald M.; Gardeniers, Johannes G.E.; Lefferts, Leonardus

    2012-01-01

    In this work the applicability of X-ray fluorescence spectroscopy (XRF) for fast, accurate and non-destructive determination of the thickness of a variety of single-layer and multi-layer metal thin films deposited on glass and silicon is investigated. Data obtained with XRF is compared with

  5. Characterization of contaminated soils using a x-ray fluorescence equipment; Caracterizacion de suelos contaminados mediante un equipo portatil de fluorescencia de rayos X

    Energy Technology Data Exchange (ETDEWEB)

    Quindos, L. S.; Fuente, I.; Sainz, C.; Queral, I.

    2006-07-01

    Fast and accurate material identification is required in many areas of the metal industry as well as surveillance of contaminated areas. The portable X-ray analyzer described in this paper consists of a hand-held probe and electronic unit. The system is configured with three excitation sources, such as ''241 Am, ''109Cd and ''55 Fe, which provides excellent performance for common elements to be controlled in contaminated soils. Data about measurements developed with this device in field as well as in the laboratory are shown in this paper. (Author)

  6. Trace elements as tumor biomarkers and prognostic factors in breast cancer: a study through energy dispersive x-ray fluorescence

    Science.gov (United States)

    2012-01-01

    Background The application and better understanding of traditional and new breast tumor biomarkers and prognostic factors are increasing due to the fact that they are able to identify individuals at high risk of breast cancer, who may benefit from preventive interventions. Also, biomarkers can make possible for physicians to design an individualized treatment for each patient. Previous studies showed that trace elements (TEs) determined by X-Ray Fluorescence (XRF) techniques are found in significantly higher concentrations in neoplastic breast tissues (malignant and benign) when compared with normal tissues. The aim of this work was to evaluate the potential of TEs, determined by the use of the Energy Dispersive X-Ray Fluorescence (EDXRF) technique, as biomarkers and prognostic factors in breast cancer. Methods By using EDXRF, we determined Ca, Fe, Cu, and Zn trace elements concentrations in 106 samples of normal and breast cancer tissues. Cut-off values for each TE were determined through Receiver Operating Characteristic (ROC) analysis from the TEs distributions. These values were used to set the positive or negative expression. This expression was subsequently correlated with clinical prognostic factors through Fisher’s exact test and chi-square test. Kaplan Meier survival curves were also evaluated to assess the effect of the expression of TEs in the overall patient survival. Results Concentrations of TEs are higher in neoplastic tissues (malignant and benign) when compared with normal tissues. Results from ROC analysis showed that TEs can be considered a tumor biomarker because, after establishing a cut-off value, it was possible to classify different tissues as normal or neoplastic, as well as different types of cancer. The expression of TEs was found statistically correlated with age and menstrual status. The survival curves estimated by the Kaplan-Meier method showed that patients with positive expression for Cu presented a poor overall survival (p

  7. X-ray fluorescence analysis with micro glass beads using milligram-scale siliceous samples for archeology and geochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Ichikawa, Shintaro, E-mail: sichi@meiji.ac.jp [Organization for the Strategic Coordination of Research and Intellectual Properties, Meiji University, Kawasaki 214-8571 (Japan); Nakamura, Toshihiro [Department of Applied Chemistry, Meiji University, Kawasaki 214-8571 (Japan)

    2014-06-01

    A micro glass bead technique was developed to assay precious siliceous samples for geochemical and archeological analyses. The micro-sized (approximately 3.5 mm in diameter and 0.8 mm in height) glass beads were prepared by mixing and fusing 1.1 mg of the powdered sample and 11.0 mg of the alkali lithium tetraborate flux for wavelength-dispersive X-ray fluorescence determination of major oxides (Na{sub 2}O, MgO, Al{sub 2}O{sub 3}, SiO{sub 2}, P{sub 2}O{sub 5}, K{sub 2}O, CaO, TiO{sub 2}, MnO, and total Fe{sub 2}O{sub 3}). The preparation parameters, including temperature and agitation during the fusing process, were optimized for the use of a commercial platinum crucible rather than a custom-made crucible. The procedure allows preparation of minute sample amounts of siliceous samples using conventional fusing equipment. Synthetic calibration standards were prepared by compounding chemical reagents such as oxides, carbonates, and diphosphates. Calibration curves showed good linearity with r values > 0.997, and the lower limits of detection were in the 10s to 100s of μg g{sup −1} range (e.g., 140 μg g{sup −1} for Na{sub 2}O, 31 μg g{sup −1} for Al{sub 2}O{sub 3}, and 8.9 μg g{sup −1} for MnO). Using the present method, we determined ten major oxides in igneous rocks, stream sediments, ancient potteries, and obsidian. This was applicable to siliceous samples with various compositions, because of the excellent agreement between the analytical and recommended values of six geochemical references. This minimal-scale analysis may be available for precious and limited siliceous samples (e.g., rock, sand, soil, sediment, clay, and archeological ceramics) in many fields such as archeology and geochemistry. - Highlights: • X-ray fluorescence determination of major oxides was performed using 1.1 mg of sample. • Preparation and measurement techniques of the XRF micro glass bead specimen were optimized. • Calibration curves using synthetic standards showed good

  8. Quantitative 3D elemental analysis inside plant roots by means of synchrotron confocal micro X-ray fluorescence

    Science.gov (United States)

    Terzano, R.; Vekemans, B.; Tomasi, N.; Spagnuolo, M.; Schoonjans, T.; Vincze, L.; Pinton, R.; Cesco, S.; Ruggiero, P.

    2009-04-01

    The knowledge of the distribution and concentration of elements within plants is a fundamental step to better understand how these plants uptake specific elements from the medium of growth and how they manage acquisition and compartmentalisation of nutrients as well as toxic metals. For some elements, either nutrients or toxicants, it can be of relevance to know their concentration level within microscopic volumes in plant organs, where they are stored or accumulated. Usually, this type of microscopic analysis requires complex cutting procedures and extensive sample manipulations. In this research, the technique of synchrotron micro X-ray fluorescence in the confocal mode was applied to image the distribution of elements in selected key-planes of tomato roots without the need of any sample preparation, except washing and freeze-drying. Using this method, a first polycapillary lens focussed the X-ray beam with an energy of 12.4 keV down to a 20 µm beam that is penetrating the sample, and a second polycapillary half-lens, that was positioned at the detection side at 90 degrees to the first polycapillary, could then restrict further the view on this irradiated volume to a defined microscopic volume (typically 20x20x20 µm3) from which the induced fluorescent radiation is finally collected by the energy dispersive detector. In this way, it was possible to investigate the concentration levels of some elements such as K, Ca, Mn, Fe, Cu and Zn within the roots of tomato plants. The quantification was performed by means of a dedicated XRF Fundamental Parameter (FP) method in order to calculate the concentrations of trace elements within the analysed plants. Utilizing fundamental atomic parameters, the applied FP method is taking into account the influence of sample self-absorption and especially the specific detection processes by the polycapillary lens. Quantification was assessed and validated by using different standards: NIST SRM 1573a (trace elements in tomato leaves

  9. X-Ray Fluorescence Spectrometry. II Determination of Uranium in ores; Espectrometria de fluorescencia de Rayos X. II-Aplicacion a la determinacion de uranio en minerales

    Energy Technology Data Exchange (ETDEWEB)

    Bermudez Polonio, J.; Crus Castillo, F. de la; Fernandez Cellini, R.

    1961-07-01

    A method of analysis of uranium in ores by X-ray spectrometry was developed, using the internal standard technique. Strontium was found to be the most suitable internal standard for general use. A Norelco Philips X-ray fluorescent spectrometer was used in this work, equipped with a lithium fluoride crystal acting as a diffraction grating analyzer. The intensity of the uranium-L {alpha}{sub 1} spectral line is calculated and related to corresponding strontium-K{sub {alpha}} spectral line, both detected with a Scintillation Counter. (Author) 31 refs.

  10. X-ray fluorescence holographic study on high-temperature superconductor FeSe{sub 0.4}Te{sub 0.6}

    Energy Technology Data Exchange (ETDEWEB)

    Ideguchi, Yuki; Kamimura, Kenji; Kimura, Koji [Kumamoto Univ. (Japan). Dept. of Physics; and others

    2016-07-01

    To observe the difference of atomic heights between the Se and Te layers with respect to the Fe layer in FeSe{sub 0.4}Te{sub 0.6} single crystal, a Fe Kα fluorescence X-ray holography (XFH) experiment was performed at room temperature. The crystal structure of superconductor FeSe{sub 0.4}Te{sub 0.6} obtained by X-ray diffraction (XRD) at a low temperature has distinct z-coordinates of Se and Te, remarkably different from each other. The reconstructed atomic image around central Fe atoms by XFH, however, reveals the different and complex results.

  11. Optical molecular imaging-guided radiation therapy part 2: Integrated x-ray and fluorescence molecular tomography.

    Science.gov (United States)

    Shi, Junwei; Udayakumar, Thirupandiyur S; Wang, Zhiqun; Dogan, Nesrin; Pollack, Alan; Yang, Yidong

    2017-09-01

    Differentiating tumor from its surrounding soft tissues is challenging for x-ray computed tomography (CT). Fluorescence molecular tomography (FMT) can directly localize the internal tumors targeted with specific fluorescent probes. A FMT system was developed and integrated onto a CT-guided irradiator to improve tumor localization for image-guided radiation. The FMT system was aligned orthogonal to the cone-beam CT onboard our previously developed image-guided small animal arc radiation treatment system (iSMAART). Through rigorous physical registration, the onboard CT provides accurate surface contour which is used to generate three-dimensional mesh for FMT reconstruction. During FMT experiments, a point laser source perpendicular to the rotating axis was used to excite the internal fluorophores. The normalized optical images from multiple projection angles were adopted for tomographic reconstruction. To investigate the accuracy of the FMT in locating the tumor and recovering its volume, in vivo experiments were conducted on two breast cancer models: MDA-MB-231 cancer xenograft on nude mice and 4T1 cancer xenograft on white mice. Both cancer cell lines overexpress the epidermal growth factor receptor (EGFR). A novel fluorescent poly(lactic-co-glycolic) acid (PLGA) nanoparticle conjugated with anti-EGFR was intravenously injected to specifically target the breast cancer cells. Another ex vivo experiment on a mouse bearing a surgically implanted Indocyanine Green-containing glass tube was conducted, to additionally validate the precision of FMT-guided radiation therapy. The FMT can accurately localize the single-nodule breast tumors actively targeted with fluorescent nanoparticles with localization error FMT and CT. The reconstructed tumor volume in FMT was significantly correlated with that in the iodinated contrast-enhanced CT (R2 = 0.94, P FMT was able to guide focal radiation delivery with submillimeter accuracy. Using the tumor-targeting fluorescent probes, the i

  12. Localization of iron in rice grain using synchrotron X-ray fluorescence microscopy and high resolution secondary ion mass spectrometry

    KAUST Repository

    Kyriacou, Bianca

    2014-03-01

    Cereal crops accumulate low levels of iron (Fe) of which only a small fraction (5-10%) is bioavailable in human diets. Extensive co-localization of Fe in outer grain tissues with phytic acid, a strong chelator of metal ions, results in the formation of insoluble complexes that cannot be digested by humans. Here we describe the use of synchrotron X-ray fluorescence microscopy (XFM) and high resolution secondary ion mass spectrometry (NanoSIMS) to map the distribution of Fe, zinc (Zn), phosphorus (P) and other elements in the aleurone and subaleurone layers of mature grain from wild-type and an Fe-enriched line of rice (Oryza sativa L.). The results obtained from both XFM and NanoSIMS indicated that most Fe was co-localized with P (indicative of phytic acid) in the aleurone layer but that a small amount of Fe, often present as "hotspots", extended further into the subaleurone and outer endosperm in a pattern that was not co-localized with P. We hypothesize that Fe in subaleurone and outer endosperm layers of rice grain could be bound to low molecular weight chelators such as nicotianamine and/or deoxymugineic acid. © 2014.

  13. Trace elements determination by energy dispersive X-ray fluorescence (EDXRF) in human placenta and membrane: a comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Custodio, P.J.; Carvalho, M.L. [Centro Fisica Atomica, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003, Lisboa (Portugal); Nunes, F. [Hospital Garcia de Orta, Almada (Portugal)

    2003-04-01

    This work is an application of energy dispersive X-ray fluorescence (EDXRF) as an analytical technique for trace elemental determination in human membrane and placenta and elemental concentrations correlations in both tissues. Whole samples were collected during the delivery from healthy mothers and full-term pregnancies. The age of the mother was between 25 and 40 years old, and the weight of the infants ranged from 2.56 to 4.05 kg. Samples were lyophilised and analysed without any chemical treatment. No significant differences in elemental content of placenta and membrane samples were observed except for Ca. Very low levels of Se, As and Pb were observed in all the analysed samples. Zn, considered as one of the key elements in newborn health, was not significantly different in the analysed samples, all of which originated from healthy mothers and healthy babies. The obtained values agree with the literature except for Ca, which is much higher in the studied samples. (orig.)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-09-15

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

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

    Science.gov (United States)

    Vázquez, Cristina; Custo, Graciela; Barrio, Néstor; Burucúa, José; Boeykens, Susana; Marte, Fernando

    2010-09-01

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

  16. Performance evaluation of currently used portable X ray fluorescence instruments for measuring the lead content of paint in field samples.

    Science.gov (United States)

    Muller, Yan; Favreau, Philippe; Kohler, Marcel

    2014-01-01

    Field-portable X-ray fluorescence (FP-XRF) instruments are important for non-destructive, rapid and convenient measurements of lead in paint, in view of potential remediation. Using real-life paint samples, we compared measurements from three FP-XRF instruments currently used in Switzerland with laboratory measurements using inductively coupled plasma mass spectrometry after complete sample dissolution. Two FP-XRF devices that functioned by lead L shell excitation frequently underestimated the lead concentration of samples. Lack of accuracy correlated with lead depth and/or the presence of additional metal elements (Zn, Ba or Ti). A radioactive source emitter XRF that enabled the additional K shell excitation showed higher accuracy and precision, regardless of the depth of the lead layer in the sample or the presence of other elements. Inspection of samples by light and electron microscopy revealed the diversity of real-life samples, with multi-layered paints showing various depths of lead and other metals. We conclude that the most accurate measurements of lead in paint are currently obtained with instruments that provide at least sufficient energy for lead K shell excitation.

  17. [Use of radionuclide x-ray fluorescence analysis in pharmacy practice--determination of levels of elements in pharmaceutic aids].

    Science.gov (United States)

    Sýkorová, M; Havránek, E

    2003-07-01

    X-ray fluorescence analysis (XRF) has been employed for the identification and determination of elements with Z > 18. In pharmacy, it can be used to determine the content of elements in drugs and pharmaceutical auxiliary substances. The method makes it possible to distinguish heavy metals in the tests of purity of drugs. It can also be used to verify the origin of the raw material or drug on the basis of its elemental composition. The present paper is concerned with the preparation of samples of pharmaceutical auxiliary substances for the determination of the content of the elements Fe, Cu, Zn, and Pb by the XRF method with the use of a radionuclide source of 238Pu. For the determination of the content of elements, three kinds of standards were prepared aiming to remove the effect of absorption properties of the sample. The results with statistical evaluations of precision of measurement are tabulated. The study carried out an analysis of 7 samples of fillers, 3 samples of gelatine, 2 samples of SILOXID, and 1 sample of AEROSIL.

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

    Science.gov (United States)

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

    2018-03-01

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

  19. Manganese accumulates within golgi apparatus in dopaminergic cells as revealed by synchrotron X-ray fluorescence nanoimaging.

    Science.gov (United States)

    Carmona, Asunción; Devès, Guillaume; Roudeau, Stéphane; Cloetens, Peter; Bohic, Sylvain; Ortega, Richard

    2010-03-17

    Chronic exposure to manganese results in neurological symptoms referred to as manganism and is identified as a risk factor for Parkinson's disease. In vitro, manganese induces cell death in the dopaminergic cells, but the mechanisms of manganese cytotoxicity are still unexplained. In particular, the subcellular distribution of manganese and its interaction with other trace elements needed to be assessed. Applying synchrotron X-ray fluorescence nanoimaging, we found that manganese was located within the Golgi apparatus of PC12 dopaminergic cells at physiologic concentrations. At increasing concentrations, manganese accumulates within the Golgi apparatus until cytotoxic concentrations are reached resulting in a higher cytoplasmic content probably after the Golgi apparatus storage capacity is exceeded. Cell exposure to manganese and brefeldin A, a molecule known to specifically cause the collapse of the Golgi apparatus, results in the striking intracellular redistribution of manganese, which accumulates in the cytoplasm and the nucleus. These results indicate that the Golgi apparatus plays an important role in the cellular detoxification of manganese. In addition manganese exposure induces a decrease in total iron content, which could contribute to the overall neurotoxicity.

  20. X-ray Fluorescence analytical criteria to assess the fineness of ancient silver coins: Application on Ptolemaic coinage

    Energy Technology Data Exchange (ETDEWEB)

    Kantarelou, Vasiliki, E-mail: kantarelou@inp.demokritos.gr [Institute of Nuclear Physics, NCSR ' Demokritos' , Aghia Paraskevi Attikis, 153 10 (Greece); Ager, Francisco Jose, E-mail: fjager@us.es [Departamento de Fisica Aplicada I, Universidad de Sevilla, Sevilla (Spain); Centro Nacional de Aceleradores, Avda. Thomas A. Edison, 7. E-41092 Sevilla (Spain); Eugenidou, Despoina [Numismatic Museum, Athens (NMA), Athens (Greece); Chaves, Francisca [Departamento de Prehistoria y Arqueologia, Universidad de Sevilla, Sevilla (Spain); Andreou, Alexandros; Kontou, Elena; Katsikosta, Niki [Numismatic Museum, Athens (NMA), Athens (Greece); Respaldiza, Miguel Angel [Departamento de Fisica Aplicada I, Universidad de Sevilla, Sevilla (Spain); Serafin, Patrizia [Dipartimento di Beni Culturali, Musica e Spettacolo, Universita degli Studi di Roma ' Tor Vergata' , Roma (Italy); Sokaras, Dimosthenis [Institute of Nuclear Physics, NCSR ' Demokritos' , Aghia Paraskevi Attikis, 153 10 (Greece); Zarkadas, Charalambos [PANalytical B.V., 7600 AA Almelo (Netherlands); Polikreti, Kyriaki, E-mail: kpolykreti@culture.gr [Hellenic Ministry of Culture, Directorate of Conservation of Ancient and Modern Monuments, Dept. of Applied Research, Pireos 81, 105 53, Athens (Greece); Karydas, Andreas Germanos, E-mail: A.Karydas@iaea.org [Institute of Nuclear Physics, NCSR ' Demokritos' , Aghia Paraskevi Attikis, 153 10 (Greece); Nuclear Spectrometry and Applications Laboratory, IAEA, Seibersdorf (Austria)

    2011-09-15

    The application of X-ray Fluorescence (XRF) analysis in a non-invasive manner on ancient silver coins may not provide reliable bulk compositional data due to possible presence of a surface, silver enriched layer. The present work proposes a set of three complementary analytical methodologies to assess and improve the reliability of XRF data in such cases: a) comparison of XRF data on original and cleaned micro-spots on coin surface, b) Ag K/L ratio test and c) comparison of experimental and theoretically simulated intensities of the Rayleigh characteristic radiation emitted from the anode. The proposed methodology was applied on 82 silver coins from the collection of Ioannes Demetriou, donated to the Numismatic Museum of Athens in the 1890s. The coins originate from different mints and are attributed to the first five Ptolemaic kings' reign (321-180 B.C.). They were analyzed in-situ by using a milli-probe XRF spectrometer. The presence of an Ag-enriched layer was excluded for the majority of them. The silver fineness was found to be high, with very low concentrations of copper and lead. The composition data provide important information about possible sources of silver during the Ptolemaic period and indications of a gradual coinage debasement after 270 B.C. due to economic or technical reasons.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-06-15

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

  2. Distribution of toxic elements in teeth treated with amalgam using μ-energy dispersive X-ray fluorescence

    Science.gov (United States)

    Guerra, M.; Ferreira, C.; Carvalho, M. L.; Santos, J. P.; Pessanha, S.

    2016-08-01

    Over the years, the presence of mercury in amalgam fillings has raised some safety concerns. Amalgam is one of the most commonly used tooth fillings and contains approximately 50% of elemental mercury and 50% of other metals, mostly silver, tin and copper. Amalgam can release small amounts of mercury vapor over time, and patients can absorb these vapors by inhaling or ingesting them. In this study, 10 human teeth treated with dental amalgam were analyzed using energy dispersive X-ray fluorescence (EDXRF) to study the diffusion of its constituents, Ag, Cu, Sn and Hg. The used EDXRF setup, makes use of a polycapillary lens to focus radiation up to 25 μm allowing the mapping of the elemental distribution in the samples. Quantification was performed using the inbuilt software based on the Fundamental Parameters method for bulk samples, considering a hydroxyapatite matrix. The teeth were longitudinally cut and each slice was scanned from the surface enamel to the inner region (dentin and pulp cavity). Mercury concentration profiles show strong levels of this element close to the amalgam region, decreasing significantly in the dentin, and increasing again up to 40,000 μg·g- 1 in the cavity were the pulp used to exist when the tooth was vital.

  3. Relative accuracy testing of an X-ray fluorescence-based mercury monitor at coal-fired boilers

    Energy Technology Data Exchange (ETDEWEB)

    K. James Hay; Bruce E. Johnsen; Paul R. Ginochio; John A. Cooper [U.S. Army Engineer Research and Development Center, Champaign, IL (United States). Construction Engineering Research Laboratory

    2006-05-15

    The relative accuracy (RA) of a newly developed mercury continuous emissions monitor, based on X-ray fluorescence, was determined by comparing analysis results at coal-fired plants with two certified reference methods (American Society for Testing and Materials (ASTM) Method D6784-02 and U.S. Environment Protection Agency (EPA) Method 29). During the first determination, the monitor had an RA of 25% compared with ASTM Method D6784-02 (Ontario Hydro Method). However, the Ontario Hydro Method performed poorly, because the mercury concentrations were near the detection limit of the reference method. The mercury in this exhaust stream was primarily elemental. The second test was performed at a U.S. Army boiler against EPA Reference Method 29. Mercury and arsenic were spiked because of expected low mercury concentrations. The monitor had an RA of 16% for arsenic and 17% for mercury, meeting RA requirements of EPA Performance Specification 12a. The results suggest that the sampling stream contained significant percentages of both elemental and oxidized mercury. The monitor was successful at measuring total mercury in particulate and vapor forms. 25 refs., 8 figs., 3 tabs.

  4. Rapid and accurate analyses of silicon and phosphorus in plants using a portable X-ray fluorescence spectrometer.

    Science.gov (United States)

    Reidinger, Stefan; Ramsey, Michael H; Hartley, Susan E

    2012-08-01

    The elemental analysis of plant material is a frequently employed tool across biological disciplines, yet accurate, convenient and economical methods for the determination of some important elements are currently lacking. For instance, digestion-based techniques are often hazardous and time-consuming and, particularly in the case of silicon (Si), can suffer from low accuracy due to incomplete solubilization and potential volatilization, whilst other methods may require large, expensive and specialised equipment. Here, we present a rapid, safe and accurate procedure for the simultaneous, nonconsumptive analysis of Si and phosphorus (P) in as little as 0.1 g dried and ground plant material using a portable X-ray fluorescence spectrometer (P-XRF). We used certified reference materials from different plant species to test the analytical performance of P-XRF and show that the analysis suffers from very little bias and that the repeatability precision of the measurements is as good as or better than that of other methods. Using this technique we were able to process and analyse 200 ground samples a day, so P-XRF could provide a particularly valuable tool for plant biologists requiring the simultaneous nonconsumptive analysis of multiple elements, including those known to be difficult to measure such as Si, in large numbers of samples. © 2012 The Authors. New Phytologist © 2012 New Phytologist Trust.

  5. A new methodology for measurement of sludge residence time distribution in a paddle dryer using X-ray fluorescence analysis.

    Science.gov (United States)

    Charlou, Christophe; Milhé, Mathieu; Sauceau, Martial; Arlabosse, Patricia

    2015-02-01

    Drying is a necessary step before sewage sludge energetic valorization. Paddle dryers allow working with such a complex material. However, little is known about sludge flow in this kind of processes. This study intends to set up an original methodology for sludge residence time distribution (RTD) measurement in a continuous paddle dryer, based on the detection of mineral tracers by X-ray fluorescence. This accurate analytical technique offers a linear response to tracer concentration in dry sludge; the protocol leads to a good repeatability of RTD measurements. Its equivalence to RTD measurement by NaCl conductivity in sludge leachates is assessed. Moreover, it is shown that tracer solubility has no influence on RTD: liquid and solid phases have the same flow pattern. The application of this technique on sludge with different storage duration at 4 °C emphasizes the influence of this parameter on sludge RTD, and thus on paddle dryer performances: the mean residence time in a paddle dryer is almost doubled between 24 and 48 h of storage for identical operating conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. A study of heavy metal pollution in Lake Victoria sediments by Energy Dispersive X-Ray Fluorescence.

    Science.gov (United States)

    Makundi, I N

    2001-01-01

    Sources of heavy metal pollution of Lake Victoria is of interest due to its economic and domestic implication in East Africa. Sediments from the shore of Lake Victoria and from some streams flowing into the lake have been analyzed for their heavy metal content using Energy Dispersive X-Ray Fluorescence (EDXRF) analysis. The samples were collected from seventeen different locations around the Municipality of Mwanza divided into three zones according to their activities. The results show that sediments from Mwanza North, which is least in anthropogenic activities, contains Cr and Co in addition to metals of terrestrial origin (K, Ca, Ti, Mn, Fe, Rb, Sr, Y, and Zr), samples from Mwanza Central, which is the town center, contains high concentrations of V, Cu, Zn and Pb, and samples collected from Mwanza South, which is the industrial area, contains the highest concentrations of V, Cu, Zn, As and Pb. It is concluded that the industrial and sewage wastes discharged into the lake are the main sources of the heavy metal contamination of Lake Victoria. Further studies will be required to assess detriments of these pollutants to human and aquatic life before policy for the factories responsible is put in place.

  7. Characterization of uranium bearing material using x-ray fluorescence and direct gamma-rays measurement techniques

    Energy Technology Data Exchange (ETDEWEB)

    Mujaini, M., E-mail: madihah@uniten.edu.my; Chankow, N. [Faculty of Engineering, Chulalongkorn University Phyathai Rd., Wang Mai, Patumwan, Bangkok 10330 (Thailand); Yusoff, M. Z.; Hamid, N. A. [College of Engineering, Universiti Tenaga Nasional 43000 Kajang, Selangor (Malaysia)

    2016-01-22

    Uranium ore can be easily detected due to various gamma-ray energies emitted from uranium daughters particularly from {sup 238}U daughters such as {sup 214}Bi, {sup 214}Pb and {sup 226}Ra. After uranium is extracted from uranium ore, only low energy gamma-rays emitted from {sup 235}U may be detected if the detector is placed in close contact to the specimen. In this research, identification and characterization of uranium bearing materials is experimentally investigated using direct measurement of gamma-rays from {sup 235}U in combination with the x-ray fluorescence (XRF) technique. Measurement of gamma-rays can be conducted by using high purity germanium (HPGe) detector or cadmium telluride (CdTe) detector while a {sup 57}Coradioisotope-excited XRF spectrometer using CdTe detector is used for elemental analysis. The proposed technique was tested with various uranium bearing specimens containing natural, depleted and enriched uranium in both metallic and powder forms.

  8. Lead detection in food, medicinal, and ceremonial items using a portable X-ray fluorescence (XRF) instrument.

    Science.gov (United States)

    Reames, Ginger; Charlton, Valerie

    2013-01-01

    The authors evaluated a Niton XLp303A X-ray fluorescence (XRF) instrument, used to identify lead hazards in housing, to determine its effectiveness to screen food, medicinal, and ceremonial items during lead poisoning investigations. Fifty-eight suspect exposure items were tested for lead by XRF and then sent to the laboratory for confirmation. A lead content cut-point of 10 parts per million (ppm; the lower level at which the XRF model could reliably determine the presence of lead) was used to evaluate the results. The Niton consistently identified the presence of lead spectra emissions and gave quantitative readings above 10 ppm for the nine samples with lead content that exceeded 10 ppm in laboratory testing. The authors' study suggests that the Niton XLp303A is an effective screening method for food and similar items with lead content > or = 10 ppm, provided the operator is trained to identify lead spectra. Rapid, on-site identification of lead exposure sources allows an investigator to inform the family of immediate steps they can take to decrease their child's lead exposure.

  9. Standard test method for determination of low concentrations of uranium in oils and organic liquids by X-ray fluorescence

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of oils and organic solutions containing uranium. Two different preparation techniques are described. 1.2 The procedure is valid for those solutions containing 20 to 2000 μg uranium per mL as presented to the spectrometer for the solution technique and 200 to 50 000 μg uranium per g for the pellet technique. 1.3 This test method requires the use of an appropriate internal standard. Care must be taken to ascertain that samples analyzed by this test method do not contain the internal standard or that this contamination, whenever present, has been corrected for mathematically. Such corrections are not addressed in this procedure. Care must be taken that the internal standard and sample medium are compatible; that is, samples must be miscible with tri-n-butyl phosphate (TBP) and must not remove the internal standard from solution. Alternatively, a scatter line may be used as the internal standard. 1....

  10. Identification of inorganic pigments used in porcelain cards based on fusing Raman and X-ray fluorescence (XRF) data.

    Science.gov (United States)

    Deneckere, Annelien; de Vries, Lieke; Vekemans, Bart; Van de Voorde, Lien; Ariese, Freek; Vincze, Laszlo; Moens, Luc; Vandenabeele, Peter

    2011-11-01

    Raman spectroscopy and X-ray fluorescence (XRF) spectroscopy are often used as complementary techniques that are well suited for the analysis of art objects because both techniques are fast, sensitive, and noninvasive and measurements can take place in situ. In most of these studies, both techniques are used separately, in the sense that the spectra are evaluated independently and single conclusions are obtained, considering both results. This paper presents a data fusion procedure for Raman and XRF data for the characterization of pigments used in porcelain cards. For the classification of the analyzed points of the porcelain cards principal component analysis (PCA) was used. A first attempt was made to develop a new procedure for the identification of the pigments using a database containing the fused Raman-XRF data of 24 reference pigments. The results show that the classification based on the fused Raman-XRF data is significantly better than the classifications based on the Raman data or the XRF data separately.

  11. Elemental analysis of granite by instrumental neutron activation analysis (INAA) and X-ray fluorescence analysis (XRF).

    Science.gov (United States)

    El-Taher, A

    2012-01-01

    The instrumental neutron activation analysis technique (INAA) was used for qualitative and quantitative analysis of granite samples collected from four locations in the Aswan area in South Egypt. The samples were prepared together with their standards and simultaneously irradiated in a neutron flux of 7×10(11)n/cm(2)s in the TRIGA Mainz research reactor. Gamma-ray spectra from an hyper-pure germanium detector were analyzed. The present study provides the basic data of elemental concentrations of granite rocks. The following elements have been determined Na, Mg, K, Fe, Mn, Sc, Cr, Ti, Co, Zn, Ga, Rb, Zr, Nb, Sn, Ba, Cs, La, Ce, Nd, Sm, Eu, Yb, Lu, Hf, Ta, Th and U. The X-ray fluorescence (XRF) was used for comparison and to detect elements, which can be detected only by XRF such as F, S, Cl, Co, Cu, Mo, Ni, Pb, Se and V. The data presented here are our contribution to understanding the elemental composition of the granite rocks. Because there are no existing databases for the elemental analysis of granite, our results are a start to establishing a database for the Egyptian granite. It is hoped that the data presented here will be useful to those dealing with geochemistry, granite chemistry and related fields. Copyright © 2011 Elsevier Ltd. All rights reserved.

  12. Fingerprinting of sildenafil citrate and tadalafil tablets in pharmaceutical formulations via X-ray fluorescence (XRF) spectrometry.

    Science.gov (United States)

    Ortiz, Rafael S; Mariotti, Kristiane C; Schwab, Nicolas V; Sabin, Guilherme P; Rocha, Werickson F C; de Castro, Eustáquio V R; Limberger, Renata P; Mayorga, Paulo; Bueno, Maria Izabel M S; Romão, Wanderson

    2012-01-25

    The production of counterfeited drugs is a criminal problem that carries serious risks to public health in the worldwide. In Brazil, Viagra and Cialis are the most counterfeit medicines, being used to inhibit the phosphodiesterase type 5 (PDE-5), treating thus, problems related to erectile dysfunction. X-ray fluorescence (XRF) is a suitable technique to control the quality of new pharmaceutical formulations and distinguish between authentic and counterfeit tablets. XRF has advantageous features like multielemental capability, good detectivity, high precision, short analysis times, and is nondestructive, which makes it suitable to be extended to a great variety of samples. In this work, the inorganic fingerprinting chemical of forty-one commercial samples (Viagra, Cialis, Lazar, Libiden, Maxfil, Plenovit, Potent 75, Rigix, V-50, Vimax and Pramil) and fifty-six counterfeit samples (Viagra and Cialis) were obtained from XRF data. XRF presented an excellent analytical methodology for semi-quantitative determination of active ingredient (in case of sildenafil citrate that presents S in its structure) and excipients such as calcium phosphate, titanium oxide and iron oxide (P, Ca, Ti and Fe). The matrix data were allied to chemometric methods (Principal Component Analysis and Hierarchical Cluster Analysis) to classify the tablets investigated between authentic and counterfeit, grouping the samples into of seven groups: A, B, C, D and E (counterfeit group) and F and G (authentic group). Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

  13. A novel total reflection X-ray fluorescence procedure for the direct determination of trace elements in petrochemical products

    Energy Technology Data Exchange (ETDEWEB)

    Cinosi, Amedeo [Sasol Italy SpA, Paderno Dugnano (Italy); GNR srl, Agrate Conturbia, Novara (Italy); Andriollo, Nunzio [Sasol Italy SpA, Paderno Dugnano (Italy); Pepponi, Giancarlo [Fondazione Bruno Kessler, Povo, Trento (Italy); Monticelli, Damiano [Universita degli Studi dell' Insubria - sede di Como, Dipartimento di Scienze Chimiche e Ambientali, Como, CO (Italy)

    2011-01-15

    A total reflection X-ray fluorescence (TXRF) procedure was developed for the determination of metal traces in petrochemical end products or intermediates for surfactant synthesis. The method combines a fast and straightforward sample preparation, i.e. deposition on the sample holder and evaporation of the sample matrix, with an efficient quantification method based on internal standardization (organic gallium standard). The method developed showed detection limits below 0.05 {mu}g g{sup -1} and in most cases below 0.005 {mu}g g{sup -1}. Fifteen elements (Ca, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Rh, Sn, Sr, V and Zn) were determined in matrices such as paraffins, n-olefins, linear alkylbenzenes, long-chain alkyl alcohols and esters: typical metal contents were below 1 {mu}g g{sup -1}. The results were compared with the reference method ASTM D5708 (test method B) based on inductively coupled plasma optical emission spectroscopy: advantages and drawbacks of the two procedures were critically evaluated. The TXRF method developed showed comparable precision and absence of bias with respect to the reference method. A comparison of the performances of the two methods is presented. (orig.)

  14. Energy dispersive X-ray fluorescence analysis of mine waters from the Migori Gold Mining Belt in Southern Nyanza, Kenya.

    Science.gov (United States)

    Odumo, O B; Mustapha, A O; Patel, J P; Angeyo, H K

    2011-09-01

    Analyses of water samples from Mikei, Osiri, Masara and Macalder (Makalda) gold mines of the Migori gold mining belt of Southwestern Kenya were done to determine the level of heavy metals using the Energy Dispersive X-ray Fluorescence technique. The concentrations of the heavy metals were; copper (29.34 ± 5.01-14,975.59 ± 616.14 μg/L); zinc (33.69 ± 4.29-683.15 ± 32.93 μg/L); arsenic (958.16 ± 60.14-18,047.52 ± 175.00 μg/L) and lead (19.51 ± 5.5-214.53 ± 6.29 μg/L). High levels of arsenic and lead were noted. These heavy metals are not only dangerous to the lives of miners and the local inhabitants; they are also a threat to aquatic life since these waters finally find their way into Lake Victoria.

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

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, D.; Gerwinski, W.; Radke, I. (Bundesamt fuer Seeschiffahrt und Hydrographie, Hamburg (Germany))

    1993-02-01

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

  16. Standard test method for analysis of uranium and thorium in soils by energy dispersive X-Ray fluorescence spectroscopy

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the energy dispersive X-ray fluorescence (EDXRF) spectrochemical analysis of trace levels of uranium and thorium in soils. Any sample matrix that differs from the general ground soil composition used for calibration (that is, fertilizer or a sample of mostly rock) would have to be calibrated separately to determine the effect of the different matrix composition. 1.2 The analysis is performed after an initial drying and grinding of the sample, and the results are reported on a dry basis. The sample preparation technique used incorporates into the sample any rocks and organic material present in the soil. This test method of sample preparation differs from other techniques that involve tumbling and sieving the sample. 1.3 Linear calibration is performed over a concentration range from 20 to 1000 μg per gram for uranium and thorium. 1.4 The values stated in SI units are to be regarded as the standard. The inch-pound units in parentheses are for information only. 1.5 This standard...

  17. X-ray Fluorescence analytical criteria to assess the fineness of ancient silver coins: Application on Ptolemaic coinage

    Science.gov (United States)

    Kantarelou, Vasiliki; Ager, Francisco José; Eugenidou, Despoina; Chaves, Francisca; Andreou, Alexandros; Kontou, Elena; Katsikosta, Niki; Respaldiza, Miguel Angel; Serafin, Patrizia; Sokaras, Dimosthenis; Zarkadas, Charalambos; Polikreti, Kyriaki; Karydas, Andreas Germanos

    2011-09-01

    The application of X-ray Fluorescence (XRF) analysis in a non-invasive manner on ancient silver coins may not provide reliable bulk compositional data due to possible presence of a surface, silver enriched layer. The present work proposes a set of three complementary analytical methodologies to assess and improve the reliability of XRF data in such cases: a) comparison of XRF data on original and cleaned micro-spots on coin surface, b) Ag K/L ratio test and c) comparison of experimental and theoretically simulated intensities of the Rayleigh characteristic radiation emitted from the anode. The proposed methodology was applied on 82 silver coins from the collection of Ioannes Demetriou, donated to the Numismatic Museum of Athens in the 1890s. The coins originate from different mints and are attributed to the first five Ptolemaic kings' reign (321-180 B.C.). They were analyzed in-situ by using a milli-probe XRF spectrometer. The presence of an Ag-enriched layer was excluded for the majority of them. The silver fineness was found to be high, with very low concentrations of copper and lead. The composition data provide important information about possible sources of silver during the Ptolemaic period and indications of a gradual coinage debasement after 270 B.C. due to economic or technical reasons.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-01

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

  19. The analysis of thallium in geological materials by radiochemical neutron activation and x-ray fluorescence spectrometry: a comparison

    Energy Technology Data Exchange (ETDEWEB)

    McGoldrick, P.J.; Robinson, P. [Tasmania Univ., Sandy Bay, TAS (Australia)

    1993-12-31

    Carrier-based radiochemical neutron activation (RNAA) is a precise and accurate technique for the analysis of Tl in geological materials. For about a decade, until the mid-80s, a procedure modified from Keays et al. (1974) was used at the University of Melbourne to analyse for Tl in a wide variety of geological materials. Samples of powdered rock weighing several hundred milligrams each were irradiated in HIFAR for between 12 hours and 1 week, and subsequently fused with a sodium hydroxide - sodium peroxide mixture and several milligrams of inactive Tl carrier. Following acid digestion of the fusion mixture anion exchange resin was used to separate Tl from the major radioactive rock constituents. The Tl was then stripped from the resin and purified as thallium iodide and a yield measured gravimetrically. Activity from {sup 204}Tl (a {beta}-emitter with a 3 8 year half-life) was measured and Tl determined by reference to pure chemical standards irradiated and processed along with the unkowns. Detection limits for the longer irradiations were about one part per billion. Precision was monitored by repeat analyses of `internal standard` rocks and was estimated to be about five to ten percent (one standard deviation). On the other hand, X-ray fluorescence spectrometry (XRF) was seen as an excellent cost-effective alternative for thallium analysis in geological samples, down to 1 ppm. 6 refs. 1 tab., 1 fig.

  20. X-ray induced fluorescence measurement of segregation in a DyI3 Hg metal-halide lamp

    Science.gov (United States)

    Nimalasuriya, T.; Curry, J. J.; Sansonetti, C. J.; Ridderhof, E. J.; Shastri, S. D.; Flikweert, A. J.; Stoffels, W. W.; Haverlag, M.; van der Mullen, J. J. A. M.

    2007-05-01

    Segregation of elemental Dy in a DyI3-Hg metal-halide high-intensity discharge lamp has been observed with x-ray induced fluorescence. Significant radial and axial Dy segregation are seen, with the axial segregation characterized by a Fischer parameter value of λ = 0.215 ± 0.002 mm-1. This is within 7% of the value (λ = 0.20 ± 0.01 mm-1) obtained by Flikweert et al (2005 J. Appl. Phys. 98 073301) based on laser absorption by neutral Dy atoms. Elemental I is seen to exhibit considerably less axial and radial segregation. Some aspects of the observed radial segregation are compatible with a simplified fluid picture describing two main transition regions in the radial coordinate. The first transition occurs in the region where DyI3 molecules are in equilibrium with neutral Dy atoms. The second transition occurs where neutral Dy atoms are in equilibrium with ionized Dy. These measurements are part of a larger study on segregation in metal-halide lamps under a variety of conditions.

  1. Analytical capabilities of total reflection X-ray fluorescence spectrometry for silver nanoparticles determination in soil adsorption studies

    Science.gov (United States)

    Torrent, Laura; Iglesias, Mònica; Hidalgo, Manuela; Marguí, Eva

    2016-12-01

    In recent years, the production of silver nanoparticles (AgNPs) has grown due to their antibacterial properties. This fact enhances the release of these particles into the environment, especially in soils that are the major sink. To better understand adsorption processes in soils, usually batch kinetic studies are carried out. In this context, we tested the possibilities of using total reflection X-ray fluorescence spectrometry (TXRF) to monitor the silver content in soil adsorption kinetic studies. It was found that the lower limit of detection for Ag (through Ag-Kα detection) in aqueous solutions was around 37 μg·L- 1, which was suitable to carry out this kind of studies. Moreover, the direct analysis of Ag adsorbed onto soil after the kinetic studies was investigated. In this case, the limit of detection for Ag was around 1.7 mg·kg- 1. All TXRF results were compared with those obtained by inductively coupled plasma optic emission spectrometry and good agreement was found. The batch adsorption tests performed showed that 98% of polyvinylpyrrolidone coated AgNPs were retained on the tested soils in < 6 h.

  2. Threshold for ion movements in wood cell walls below fiber saturation observed by X-ray fluorescence microscopy (XFM)

    Energy Technology Data Exchange (ETDEWEB)

    Zelinka, Samuel L.; Gleber, Sophie-Charlotte; Vogt, Stefan; Rodriguez Lopez, Gabriela M.; Jakes, Joseph E.

    2015-05-01

    Diffusion of chemicals and ions through the wood cell wall plays an important role in wood damage mechanisms. In the present work, free diffusion of ions through wood secondary walls and middle lamellae has been investigated as a function of moisture content (MC) and anatomical direction. Various ions (K, Cl, Zn, Cu) were injected into selected regions of 2 mu m thick wood sections with a microinjector and then the ion distribution was mapped by means of X-ray fluorescence microscopy with submicron spatial resolution. The MC of the wood was controlled in situ by means of climatic chamber with controlled relative humidity (RH). For all ions investigated, there was a threshold RH below which the concentration profiles did not change. The threshold RH depended upon ionic species, cell wall layer, and wood anatomical orientation. Above the threshold RH, differences in mobility among ions were observed and the mobility depended upon anatomical direction and cell wall layer. These observations support a recently proposed percolation model of electrical conduction in wood. The results contribute to understanding the mechanisms of fungal decay and fastener corrosion that occur below the fiber saturation point.

  3. Determination of heavy metals in macrozoobenthos from the rivers Tisza and Szamos by total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Woelfl, S. [Universidad Austral de Chile, Instituto de Zoologia, Casilla 567, Valdivia (Chile)]. E-mail: swoelfl@uach.cl; Mages, M. [Helmhotz Centre for Environmental Research (UFZ), Department of River Ecology, Brueckstrasse 3a, D-39114, Magdeburg (Germany); Ovari, M. [Ovari, M. Eoetvoes University, Department of Organic Chemistry, H-1117, Budapest, Pazmany P. stny. 1/a (Hungary); Geller, W. [Helmhotz Centre for Environmental Research (UFZ), Department of River Ecology, Brueckstrasse 3a, D-39114, Magdeburg (Germany)

    2006-11-15

    In 2000, accidents in the Romanian mining industry in key catchment areas led to heavy metal contamination of the Hungarian rivers Tisza and Szamos resulting in substantial heavy metal loads in several sediments of the upper river basins. This enhanced metal content might have been bioaccumulated in benthic organisms during the following years. Therefore, the aim of this study was to test, whether the zoobenthic fauna showed an enhanced metal content 3 years after the industrial accident. Macrozoobenthic insect larvae (chironomids) were sampled 100 m below and above the confluent site of the rivers Tisza and Szamos during summer 2003 and for comparison purpose also in the river Maros, a tributary of the Tisza river, during 2005. In order to determine their heavy metal content, single specimens were prepared and analysed by Total Reflection X-ray Fluorescence Spectrometry (TRXF) according to the modified dry method. Fe was much lower and Mn and Zn much higher concentrated in benthos from the more contaminated Szamos river compared to the Tisza and Maros rivers. In this sense, the benthic organisms reflected very well the enhanced metal concentrations in the contaminated rivers being suitable as bioindicators of metal contamination. However, the sediment bioaccumulation factor was low at all sampling sites indicating a low bioavailability of trace metals for benthic organisms.

  4. Synchrotron-based X-ray fluorescence microscopy enables multiscale spatial visualization of ions involved in fungal lignocellulose deconstruction

    Science.gov (United States)

    Kirker, Grant; Zelinka, Sam; Gleber, Sophie-Charlotte; Vine, David; Finney, Lydia; Chen, Si; Hong, Young Pyo; Uyarte, Omar; Vogt, Stefan; Jellison, Jody; Goodell, Barry; Jakes, Joseph E.

    2017-01-01

    The role of ions in the fungal decay process of lignocellulose biomaterials, and more broadly fungal metabolism, has implications for diverse research disciplines ranging from plant pathology and forest ecology, to carbon sequestration. Despite the importance of ions in fungal decay mechanisms, the spatial distribution and quantification of ions in lignocellulosic cell walls and fungal hyphae during decay is not known. Here we employ synchrotron-based X-ray fluorescence microscopy (XFM) to map and quantify physiologically relevant ions, such as K, Ca, Mn, Fe, and Zn, in wood being decayed by the model brown rot fungus Serpula lacrymans. Two-dimensional XFM maps were obtained to study the ion spatial distributions from mm to submicron length scales in wood, fungal hyphae with the dried extracellular matrix (ECM) from the fungus, and Ca oxalate crystals. Three-dimensional ion volume reconstructions were also acquired of wood cell walls and hyphae with ECM. Results show that the fungus actively transports some ions, such as Fe, into the wood and controls the distribution of ions at both the bulk wood and cell wall length scales. These measurements provide new insights into the movement of ions during decay and illustrate how synchrotron-based XFM is uniquely suited study these ions.

  5. X-Ray Tomographic Reconstruction

    Energy Technology Data Exchange (ETDEWEB)

    Bonnie Schmittberger

    2010-08-25

    Tomographic scans have revolutionized imaging techniques used in medical and biological research by resolving individual sample slices instead of several superimposed images that are obtained from regular x-ray scans. X-Ray fluorescence computed tomography, a more specific tomography technique, bombards the sample with synchrotron x-rays and detects the fluorescent photons emitted from the sample. However, since x-rays are attenuated as they pass through the sample, tomographic scans often produce images with erroneous low densities in areas where the x-rays have already passed through most of the sample. To correct for this and correctly reconstruct the data in order to obtain the most accurate images, a program employing iterative methods based on the inverse Radon transform was written. Applying this reconstruction method to a tomographic image recovered some of the lost densities, providing a more accurate image from which element concentrations and internal structure can be determined.

  6. The Intensity Modulation of the Fluorescent Line by a Finite Light Speed Effect in Accretion-powered X-Ray Pulsars

    Science.gov (United States)

    Yoshida, Yuki; Kitamoto, Shunji; Hoshino, Akio

    2017-11-01

    The X-ray line diagnostic method is a powerful tool for an investigation of plasma around accretion-powered X-ray pulsars. We point out an apparent intensity modulation of emission lines, with their rotation period of neutron stars, due to the finite speed of light (we call this effect the “finite light speed effect”) if the line emission mechanism is a kind of reprocessing, such as fluorescence or recombination after ionization by X-ray irradiation from pulsars. The modulation amplitude is determined by the size of the emission region, which is in competition with the smearing effect by the light crossing time in the emission region. This is efficient if the size of the emission region is roughly comparable to that of the rotation period multiplied by the speed of light. We apply this effect to a symbiotic X-ray pulsar, GX 1+4, where a spin modulation of the intense iron line of which has been reported. The finite light speed effect can explain the observed intensity modulation if its fluorescent region is the size of ˜ {10}12 cm.

  7. Validation of a hand-held X-ray absorptiometer caliper against computerized tomography for in vivo soft tissue composition analysis

    Science.gov (United States)

    Objective: To develop and validate a hand-held caliper which uses a dual-energy radioactive source to monitor regional changes in mid-thigh muscle mass and % fat. Methods: Optimum photon energies were determined by minimization of uncertainties in fat content measurements due to photon count statist...

  8. Mineralogy of the clay fraction of soils from the moray cusco archaeological site: a study by energy dispersive X-ray fluorescence, X-ray diffractometry and Moessbauer spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-11-15

    The purpose of this work is to report the advances in the elemental and structural characterization of the clay fraction of soils from the terraces of the Moray Archaeological site, located 38 km north of the city of Cusco, Cusco Region. One sample was collected from each of the twelve terraces of this site and its clay fraction was separated by sedimentation. Previously the pH of the raw samples was measured resulting that all of the samples were from alkaline to strongly alkaline. Energy dispersive X-ray fluorescence (EDXRF) was used for the elemental characterization, and X-ray diffractometry (XRD) and transmission Moessbauer spectroscopy (TMS), using the {gamma} 14.4 keV nuclear resonance transition in {sup 57}Fe, were used for the structural characterization of the clays and clay minerals present in each sample. The EDXRF analyses of all the samples show the presence of relatively high concentrations of sulfur in some of the samples and relatively high concentrations of calcium in all of the samples, which may be related to the high alkalinity of the samples. By XRD it is observed the presence of quartz, calcite, gypsum, cronstedtite, 2:1 phyllosilicates, and iron oxides. The mineralogical analysis of Fe by TMS shows that it is present in the form of hematite and occupying Fe{sup 2 + } and Fe{sup 3 + } sites in phyllosilicates, cronstedtite, and other minerals not yet identified.

  9. Physical interactions of fish protamine and antisepsis peptide drugs with bacterial membranes revealed by combination of specular x-ray reflectivity and grazing-incidence x-ray fluorescence.

    Science.gov (United States)

    Abuillan, Wasim; Schneck, Emanuel; Körner, Alexander; Brandenburg, Klaus; Gutsmann, Thomas; Gill, Tom; Vorobiev, Alexei; Konovalov, Oleg; Tanaka, Motomu

    2013-07-01

    As a defined model of outer membranes of gram negative bacteria, we investigated the interaction of monolayers of lipopolysacchrides from Salmonella enterica rough strains R90 (LPS Ra) with natural and synthetic peptides. The fine structures perpendicular to the membrane plane and the ion distribution near the interface were determined by specular x-ray reflectivity (XRR) and grazing-incidence x-ray fluorescence (GIXF) in the presence and absence of divalent cations. The unique combination of XRR and GIXF allows for the quantitative identification of different modes of interactions in a high spatial resolution, which cannot be assessed by other experimental methods. Natural fish protamine disrupts the stratified membrane structures in the absence of Ca(2+) ions, while staying away from the membrane surface in the presence of Ca(2+) ions. In contrast, synthetic antisepsis peptide Pep 19-2.5 weakly adsorbs to the membrane and stays near the uncharged sugar units even in the absence of Ca(2+). In the presence of Ca(2+), Pep 19-2.5 can reach the negatively charged inner core without destroying the barrier capability against ions.

  10. Impact of Lipid Oxidization on Vertical Structures and Electrostatics of Phospholipid Monolayers Revealed by Combination of Specular X-ray Reflectivity and Grazing-Incidence X-ray Fluorescence.

    Science.gov (United States)

    Korytowski, Agatha; Abuillan, Wasim; Makky, Ali; Konovalov, Oleg; Tanaka, Motomu

    2015-07-30

    The influence of phospholipid oxidization of floating monolayers on the structure perpendicular to the global plane and on the density profiles of ions near the lipid monolayer has been investigated by a combination of grazing incidence X-ray fluorescence (GIXF) and specular X-ray reflectivity (XRR). Systematic variation of the composition of the floating monolayers unravels changes in the thickness, roughness and electron density of the lipid monolayers as a function of molar fraction of oxidized phospholipids. Simultaneous GIXF measurements enable one to qualitatively determine the element-specific density profiles of monovalent (K(+) or Cs(+)) and divalent ions (Ca(2+)) in the vicinity of the interface in the presence and absence of two types of oxidized phospholipids (PazePC and PoxnoPC) with high spatial accuracy (±5 Å). We found the condensation of Ca(2+) near carboxylated PazePC was more pronounced compared to PoxnoPC with an aldehyde group. In contrast, the condensation of monovalent ions could hardly be detected even for pure oxidized phospholipid monolayers. Moreover, pure phospholipid monolayers exhibited almost no ion specific condensation near the interface. The quantitative studies with well-defined floating monolayers revealed how the elevation of lipid oxidization level alters the structures and functions of cell membranes.

  11. Mineralogy of the clay fraction of soils from the moray cusco archaeological site: a study by energy dispersive X-ray fluorescence, X-ray diffractometry and Mössbauer spectroscopy

    Science.gov (United States)

    Cerón Loayza, María L.; Bravo Cabrejos, Jorge A.; Mejía Santillán, Mirian E.

    2011-11-01

    The purpose of this work is to report the advances in the elemental and structural characterization of the clay fraction of soils from the terraces of the Moray Archaeological site, located 38 km north of the city of Cusco, Cusco Region. One sample was collected from each of the twelve terraces of this site and its clay fraction was separated by sedimentation. Previously the pH of the raw samples was measured resulting that all of the samples were from alkaline to strongly alkaline. Energy dispersive X-ray fluorescence (EDXRF) was used for the elemental characterization, and X-ray diffractometry (XRD) and transmission Mössbauer spectroscopy (TMS), using the γ 14.4 keV nuclear resonance transition in 57Fe, were used for the structural characterization of the clays and clay minerals present in each sample. The EDXRF analyses of all the samples show the presence of relatively high concentrations of sulfur in some of the samples and relatively high concentrations of calcium in all of the samples, which may be related to the high alkalinity of the samples. By XRD it is observed the presence of quartz, calcite, gypsum, cronstedtite, 2:1 phyllosilicates, and iron oxides. The mineralogical analysis of Fe by TMS shows that it is present in the form of hematite and occupying Fe2 + and Fe3 + sites in phyllosilicates, cronstedtite, and other minerals not yet identified.

  12. X-ray fluorescence investigation of ordered intermetallic phases as electrocatalysts towards the oxidation of small organic molecules.

    Science.gov (United States)

    Liu, Yi; Lowe, Michael A; Finkelstein, Ken D; Dale, Darren S; DiSalvo, Francis J; Abruña, Héctor D

    2010-12-10

    The composition of ordered intermetallic nanoparticles (PtBi and PtPb) has been quantitatively studied by in situ X-ray fluorescence (XRF) during active electrochemical control in solutions of supporting electrolyte and small organic molecules (SOMs). Because the Pt L(β1,2) lines and the Bi L(α1,2) lines are only separated by 200 eV, an energy-dispersive detector and a multiple-channel analyzer (MCA) were used to record the major fluorescent emission lines from these two elements. The molar ratios of platinum to the less-noble elements (Bi, Pb) in the nanoparticles dramatically changed as a function of the applied upper limit potentials (E(ulp)) in cyclic voltammetric (CV) characterization. Similar to previous investigations for bulk intermetallic surfaces, the less-noble elements leached out from the surfaces of the intermetallic nanoparticles. For PtBi nanoparticles, the ratios of fluorescence intensities of Pt/Bi in the samples were 0.42, 0.96, and 1.36 for E(ulp)=+0.40, +0.80, and 1.20 V, respectively, while cycling the potential from -0.20 V to the E(ulp) value for 10 cycles. The leaching-out process of the less-noble elements occurred at more negative E(ulp) values than expected. After cycling to relatively positive E(ulp) values, nonuniform PtM (M=Bi of Pb) nanoparticles formed with a Pt-rich shell and intermetallic PtM core. When the supporting solutions contained active fuel molecules in addition to the intermetallic nanoparticles (formic acid for PtBi, formic acid and methanol for PtPb), kinetic stabilization effects were observed for E(ulp)=+0.80 V, in a way similar to the response of the bulk materials. It was of great importance to quantitatively explore the change in composition and structure of the intermetallic nanoparticles under active electrochemical control. More importantly, this approach represents a simple, universal, and multifunctional method for the study of multi-element nanoparticles as electrocatalysts. This is, to our knowledge, the

  13. Low-energy d-d excitations in MnO studied by resonant x-ray fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Butorin, S.M.; Guo, J.; Magnuson, M. [Uppsala Univ. (Sweden)] [and others

    1997-04-01

    Resonant soft X-ray emission spectroscopy has been demonstrated to possess interesting abilities for studies of electronic structure in various systems, such as symmetry probing, alignment and polarization dependence, sensitivity to channel interference, etc. In the present abstract the authors focus on the feasibility of resonant soft X-ray emission to probe low energy excitations by means of resonant electronic X-ray Raman scattering. Resonant X-ray emission can be regarded as an inelastic scattering process where a system in the ground state is transferred to a low excited state via a virtual core excitation. The energy closeness to a core excitation of the exciting radiation enhances the (generally) low probability for inelastic scattering at these wavelengths. Therefore soft X-ray emission spectroscopy (in resonant electronic Raman mode) can be used to study low energy d-d excitations in transition metal systems. The involvement of the intermediate core state allows one to use the selection rules of X-ray emission, and the appearance of the elastically scattered line in the spectra provides the reference to the ground state.

  14. 3D non-destructive fluorescent X-ray computed tomography (FXCT) with a CdTe array

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Chang Yeon; Lee, Won Ho; Kim, Young Hak [Dept. of Bio-convergence Engineering, Korea University Graduate School, Seoul (Korea, Republic of)

    2015-10-15

    In our research, the material was exposed to an X-ray and not only the conventional transmission image but also 3D images based on the information of characteristic X-ray detected by a 2D CdTe planar detector array were reconstructed. Since atoms have their own characteristic X-ray energy, our system was able to discriminate materials of even a same density if the materials were composed of different atomic numbers. We applied FXCT to distinguish various unknown materials with similar densities. The materials with similar densities were clearly distinguished in the 3D reconstructed images based on the information of the detected characteristic X-ray, while they were not discriminated from each other in the images based on the information of the detected transmission X-ray. In the fused images consisting of 3D transmitted and characteristic X-ray images, all of the positions, densities and atomic numbers of materials enclosed in plastic phantom or pipe were clearly identified by analyzing energy, position and amount of detected radiation.

  15. Energy dispersive X-ray fluorescence spectrometry for the direct multi-element analysis of dried blood spots

    Science.gov (United States)

    Marguí, E.; Queralt, I.; García-Ruiz, E.; García-González, E.; Rello, L.; Resano, M.

    2018-01-01

    Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients. In this sense, dried blood spots (DBS) are proposed as a non-invasive and even self-administered alternative to sampling whole venous blood. This contribution explores the potential of energy dispersive X-ray fluorescence spectrometry for the simultaneous and direct determination of some major (S, Cl, K, Na), minor (P, Fe) and trace (Ca, Cu, Zn) elements in blood, after its deposition onto clinical filter papers, thus giving rise to DBS. For quantification purposes the best strategy was to use matrix-matched blood samples of known analyte concentrations. The accuracy and precision of the method were evaluated by analysis of a blood reference material (Seronorm™ trace elements whole blood L3). Quantitative results were obtained for the determination of P, S, Cl, K and Fe, and limits of detection for these elements were adequate, taking into account their typical concentrations in real blood samples. Determination of Na, Ca, Cu and Zn was hampered by the occurrence of high sample support (Na, Ca) and instrumental blanks (Cu, Zn). Therefore, the quantitative determination of these elements at the levels expected in blood samples was not feasible. The methodology developed was applied to the analysis of several blood samples and the results obtained were compared with those reported by standard techniques. Overall, the performance of the method developed is promising and it could be used to determine the aforementioned elements in blood samples in a simple, fast and economic way. Furthermore, its non-destructive nature enables further analyses by means of complementary techniques to be carried out.

  16. Investigation of Essential Element Distribution in the Equine Metacarpophalangeal Joint using a Synchrotron Radiation Micro X-Ray Fluorescence Technique

    Science.gov (United States)

    Kaabar, Wejdan; Gundogdu, O.; Tzaphlidou, M.; Janousch, M.; Attenburrow, D.; Bradley, D. A.

    2008-05-01

    In articular cartilage, Ca, P, K and S are among some of the well known co-factors of the metalloproteinases enzymatic family, the latter playing a pivotal role in the growth and degeneration of the collagenous bone-cartilage interface of articulating joints. Current study forms part of a larger investigation concerning the distribution of these and other key elements in such media. For the purpose of evaluating these low atomic number elements (Z⩽20), use was made of the capabilities of the LUCIA Station, located at the synchrotron facility of the Paul Scherrer Institute (PSI). Using an incident radiation energy of 4.06 keV, a synchrotron radiation micro x-ray fluorescence (SR-μXRF) technique was applied in examining the distribution of the essential elements Ca, P, K and S in the bone-cartilage interface of both healthy and diseased (osteoarthritic) areas of an equine metacarpophalangeal joint. The SR-μXRF mappings and line profile patterns have revealed remarkable changes in both the pattern and absolute distributions of these elements, agreeing with the findings of others. The elemental presence shown in the individual area scans encompassing the lesion each reflect the visibly abraded outer surface of the cartilage and change in shape of the bone surface. One of the area scans for the bone-cartilage interface shows a marked change in both the pattern and absolute elemental presence for all three elements compared to that observed at two other scan sites. The observation of change in bone cartilage composition around the surface of the articulating joint is thought to be novel, the variation being almost certainly due to the differing weight-bearing role of the subchondral bone at each location.

  17. Biogenic and detrital-rich intervals in central Arctic Ocean cores identified using x-ray fluorescence scanning

    Directory of Open Access Journals (Sweden)

    Daniela Hanslik

    2013-02-01

    Full Text Available X-ray fluorescence (XRF scanning of sediment cores from the Lomonosov Ridge and the Morris Jesup Rise reveals a distinct pattern of Ca intensity peaks through Marine Isotope Stages (MIS 1 to 7. Downcore of MIS 7, the Ca signal is more irregular and near the detection limit. Virtually all major peaks in Ca coincide with a high abundance of calcareous microfossils; this is particularly conspicuous in the cores from the central Arctic Ocean. However, the recorded Ca signal is generally caused by a combination of biogenic and detrital carbonate, and in areas influenced by input from the Canadian Arctic, detrital carbonates may effectively mask the foraminiferal carbonates. Despite this, there is a strong correlation between XRF-detected Ca content and foraminiferal abundance. We propose that in the Arctic Ocean north of Greenland a common palaeoceanographic mechanism is controlling Ca-rich ice-rafted debris (IRD and foraminiferal abundance. Previous studies have shown that glacial periods are characterized by foraminfer-barren sediments. This implies that the Ca-rich IRD intervals with abundant foraminifera were most likely deposited during interglacial periods when glaciers left in the Canadian Arctic Archipelago were still active and delivered a large amount of icebergs. At the same time, conditions were favourable for planktic foraminifera, resulting in a strong covariance between these proxies. Therefore, we suggest that the XRF scanner's capability to efficiently map Ca concentrations in sediment cores makes it possible to systematically examine large numbers of cores from different regions to investigate the palaeoceanographic reasons for the calcareous microfossils’ spatial and temporal variability.

  18. First results of a novel Silicon Drift Detector array designed for low energy X-ray fluorescence spectroscopy

    Science.gov (United States)

    Rachevski, Alexandre; Ahangarianabhari, Mahdi; Bellutti, Pierluigi; Bertuccio, Giuseppe; Brigo, Elena; Bufon, Jernej; Carrato, Sergio; Castoldi, Andrea; Cautero, Giuseppe; Fabiani, Sergio; Giacomini, Gabriele; Gianoncelli, Alessandra; Giuressi, Dario; Guazzoni, Chiara; Kourousias, George; Liu, Chang; Menk, Ralf Hendrik; Montemurro, Giuseppe Vito; Picciotto, Antonino; Piemonte, Claudio; Rashevskaya, Irina; Shi, Yongbiao; Stolfa, Andrea; Vacchi, Andrea; Zampa, Gianluigi; Zampa, Nicola; Zorzi, Nicola

    2016-07-01

    We developed a trapezoidal shaped matrix with 8 cells of Silicon Drift Detectors (SDD) featuring a very low leakage current (below 180 pA/cm2 at 20 °C) and a shallow uniformly implanted p+ entrance window that enables sensitivity down to few hundreds of eV. The matrix consists of a completely depleted volume of silicon wafer subdivided into 4 square cells and 4 half-size triangular cells. The energy resolution of a single square cell, readout by the ultra-low noise SIRIO charge sensitive preamplifier, is 158 eV FWHM at 5.9 keV and 0 °C. The total sensitive area of the matrix is 231 mm2 and the wafer thickness is 450 μm. The detector was developed in the frame of the INFN R&D project ReDSoX in collaboration with FBK, Trento. Its trapezoidal shape was chosen in order to optimize the detection geometry for the experimental requirements of low energy X-ray fluorescence (LEXRF) spectroscopy, aiming at achieving a large detection angle. We plan to exploit the complete detector at the TwinMic spectromicroscopy beamline at the Elettra Synchrotron (Trieste, Italy). The complete system, composed of 4 matrices, increases the solid angle coverage of the isotropic photoemission hemisphere about 4 times over the present detector configuration. We report on the layout of the SDD matrix and of the experimental set-up, as well as the spectroscopic performance measured both in the laboratory and at the experimental beamline.

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

    Science.gov (United States)

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

    2008-12-01

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

  20. Interference-free determination of ischemia-modified albumin using quantum dot coupled X-ray fluorescence spectroscopy.

    Science.gov (United States)

    Luo, Yang; Wang, Chaoming; Jiang, Tianlun; Zhang, Bo; Huang, Junfu; Liao, Pu; Fu, Weiling

    2014-01-15

    Ischemia-modified protein (IMA) is the most sensitive diagnostic biomarker of ischemic heart disease, but differentiation of IMA from human serum albumin (HSA), a ubiquitous serum protein, is still challenging owing to the shared antigenicity. In this investigation, we developed a rapid and interference-free approach for IMA determination using quantum dots-coupled X-ray Fluorescence Spectroscopy (Q-XRF). In a typical Q-XRF assay, serum total HSA is quantified using quantum dot-coupled sandwich immunoassay, and intact HSA (iHSA) is determined using a XRF spectroscopy, by measuring XRF intensity of Co (II) bonded to iHSA. IMA concentration is automatically determined within 30 min by calculating the difference between total HSA and iHSA. This strategy can effectively eliminate the interference from native HSA level. Results show that no significant influences have been observed from hemolysis or high levels of cholesterol (7 mg/L), triglyceride (5.2 mg/L), IgG (10 g/L), and fibrinogen (4 g/L). A linearity of 1-100mg/mL is obtained in iHSA determination using XRF (r(2)=0.979). The proposed Q-XRF assay demonstrates a lowest detection limit of 0.05 U/mL. Receiver-operating characteristic (ROC) curves reveal that Q-XRF assay provide an improved sensitivity than ACB assay (95.9% vs. 82.9%) in differentiating ischemic patients from health individuals, at an optimal cutoff point of 79.2U/mL. The proposed approach provides a new strategy for interference-free, simple and rapid evaluation of IMA concentration by combining sandwich immunoassay and XRF spectroscopy. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. X-ray fluorescence microscopy reveals accumulation and secretion of discrete intracellular zinc pools in the lactating mouse mammary gland.

    Directory of Open Access Journals (Sweden)

    Nicholas McCormick

    2010-06-01

    Full Text Available The mammary gland is responsible for the transfer of a tremendous amount of zinc ( approximately 1-3 mg zinc/day from maternal circulation into milk during lactation to support the growth and development of the offspring. When this process is compromised, severe zinc deficiency compromises neuronal development and immune function and increases infant morbidity and/or mortality. It remains unclear as to how the lactating mammary gland dynamically integrates zinc import from maternal circulation with the enormous amount of zinc that is secreted into milk.Herein we utilized X-ray fluorescence microscopy (XFM which allowed for the visualization and quantification of the process of zinc transfer through the mammary gland of the lactating mouse. Our data illustrate that a large amount of zinc first accumulates in the mammary gland during lactation. Interestingly, this zinc is not cytosolic, but accumulated in large, discrete sub-cellular compartments. These zinc pools were then redistributed to small intracellular vesicles destined for secretion in a prolactin-responsive manner. Confocal microscopy identified mitochondria and the Golgi apparatus as the sub-cellular compartments which accumulate zinc; however, zinc pools in the Golgi apparatus, but not mitochondria are redistributed to vesicles destined for secretion during lactation.Our data directly implicate the Golgi apparatus in providing a large, mobilizable zinc storage pool to assist in providing for the tremendous amount of zinc that is secreted into milk. Interestingly, our study also provides compelling evidence that mitochondrial zinc pools expand in the mammary gland during lactation which we speculate may play a role in regulating mammary gland function.

  2. Soft tissue measurement of arsenic and selenium in an animal model using portable X-ray fluorescence

    Science.gov (United States)

    Fleming, David E. B.; Groves, John W.; Gherase, Mihai R.; George, Graham N.; Pickering, Ingrid J.; Ponomarenko, Olena; Langan, George; Spallholz, Julian E.; Alauddin, Mohammad; Ahsan, Habibul; Ahmed, Selim; La Porte, Paul F.

    2015-11-01

    The ingestion of trace amounts of arsenic (As) through drinking water is a relatively common pathway of exposure with potentially serious long-term health effects. Studies involving animal models have indicated that selenium (Se) may bind with As inside the body and facilitate excretion. A portable X-ray fluorescence (XRF) technique was previously developed to allow in vivo measurement of As and Se in human tissue. In the current paper, this portable XRF approach was tested for the first time using animal tissue. Seven female Lakeview Golden/LVG Syrian hamsters were dosed under either control, As-only, Se-only, or As and Se conditions. Minimum XRF detection limits in soft tissue of 1.00±0.05 ppm for As and 0.83±0.02 ppm for Se were determined from phantom calibration trials. For dosed hamsters, consistently higher concentrations of As and Se were found in the liver and gall bladder, with elevated levels also observed in the intestines. Concentrations ranged up to 26.4±1.4 ppm for As and 11.8±0.8 ppm for Se. The stomach and heart exhibited more moderate concentrations, while the brain, lung, and muscle demonstrated lower levels. For a given organ, As concentrations generally exceeded Se concentrations. A ratio of approximately 2.5:1 was observed for concentrations of As:Se when considering the same or similar tissue sites in dosed hamsters. Implications for potential in vivo human applications of the technique are briefly considered.

  3. Online X-ray Fluorescence (XRF) Analysis of Heavy Metals in Pulverized Coal on a Conveyor Belt.

    Science.gov (United States)

    Yan, Zhang; XinLei, Zhang; WenBao, Jia; Qing, Shan; YongSheng, Ling; DaQian, Hei; Da, Chen

    2016-02-01

    Heavy metals in haze episode will continue to threaten the quality of public health around the world. In order to decrease the emission of heavy metals produced from coal burning, an online X-ray fluorescence (XRF) analyzer system, consisting of an XRF analyzer with data acquisition software and a laser rangefinder, was developed to carry out the measurement of heavy metals in pulverized coal. The XRF analyzer was mounted on a sled, which can effectively smooth the surface of pulverized coal and reduce the impact of surface roughness during online measurement. The laser rangefinder was mounted over the sled for measuring the distance between a pulverized coal sample and the analyzer. Several heavy metals and other elements in pulverized coal were online measured by the XRF analyzer directly above a conveyor belt. The limits of detection for Hg, Pb, Cr, Ti, Fe, and Ca by the analyzer were 44 ± 2, 34 ± 2, 17 ± 3, 41 ± 4, 19 ± 3, and 65 ± 2 mg·kg(-1), respectively. The relative standard deviation (%RSD) for the elements mentioned was less than 7.74%. By comparison with the results by inductively-coupled plasma mass spectrometry (ICP-MS), relative deviation (%D) of the online XRF analyzer was less than 10% for Cr, Ti, and Ca, in the range of 0.8-24.26% for Fe, and greater than 20% for Hg and Pb. © The Author(s) 2016.

  4. TXRF analysis of low Z elements in serum of patients with idiopathic thrombocytopenic purpura using X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-07-01

    Idiopathic thrombocytopenic purpura (ITP) is a blood disorder characterized by an abnormal decrease in the number of platelets in the blood. ITP results from development of an antibody directed against a structural platelet antigen (an autoantibody). Platelets are also called thrombocytes, meaning cells that form clots. The cause of ITP is not known and their diagnosis requires that other disorders be excluded through selective tests. In this work, forty patients suffering from ITP and sixty healthy volunteers (Control Group) were analyzed. All the serum samples had been collected from people who live in the urban area of Rio de Janeiro City/Brazil. Blood was collected into vacutainers without additives. The measurements were performed at the X-ray fluorescence beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, Sao Paulo using a monochromatic beam with maximum energy of 20 keV for the excitation and an Ultra-LEGe detector with resolution of 148 eV at 5.9 keV. Standard solutions with Vanadium as internal standard were prepared for calibration system. It was possible to determine the elemental concentrations of the following six elements: Na, P, S, Cl, K and Ca. The Student's t-test was used to analyze significant differences ({alpha} = 0.05) between group of patients with ITP and control group. The elements that presented significant differences for the mean of their concentrations between each one of the ITP group and control group in {mu}g.g-1 were: phosphorous (136{+-}12 and 92{+-}12), Sulphur (1077{+-}97 and 847{+-}80), Chlorine (2905{+-}385 and 2266{+-}378), Potassium (137{+-}118 and 82{+-}15) and Calcium (64{+-}7 and 44{+-}6) respectively. These results will help the biomedical field with regard to early diagnosis and improved medical treatment. Thus, our findings indicate that these elements can be related to the important biochemical processes in ITP. (author)

  5. X-ray fluorescence analysis with micro glass beads using milligram-scale siliceous samples for archeology and geochemistry

    Science.gov (United States)

    Ichikawa, Shintaro; Nakamura, Toshihiro

    2014-06-01

    A micro glass bead technique was developed to assay precious siliceous samples for geochemical and archeological analyses. The micro-sized (approximately 3.5 mm in diameter and 0.8 mm in height) glass beads were prepared by mixing and fusing 1.1 mg of the powdered sample and 11.0 mg of the alkali lithium tetraborate flux for wavelength-dispersive X-ray fluorescence determination of major oxides (Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, and total Fe2O3). The preparation parameters, including temperature and agitation during the fusing process, were optimized for the use of a commercial platinum crucible rather than a custom-made crucible. The procedure allows preparation of minute sample amounts of siliceous samples using conventional fusing equipment. Synthetic calibration standards were prepared by compounding chemical reagents such as oxides, carbonates, and diphosphates. Calibration curves showed good linearity with r values > 0.997, and the lower limits of detection were in the 10s to 100s of μg g- 1 range (e.g., 140 μg g- 1 for Na2O, 31 μg g- 1 for Al2O3, and 8.9 μg g- 1 for MnO). Using the present method, we determined ten major oxides in igneous rocks, stream sediments, ancient potteries, and obsidian. This was applicable to siliceous samples with various compositions, because of the excellent agreement between the analytical and recommended values of six geochemical references. This minimal-scale analysis may be available for precious and limited siliceous samples (e.g., rock, sand, soil, sediment, clay, and archeological ceramics) in many fields such as archeology and geochemistry.

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

    Science.gov (United States)

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

    2016-02-01

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

  7. Wavelength dispersive X-ray fluorescence analysis using fundamental parameter approach of Catha edulis and other related plant samples

    Energy Technology Data Exchange (ETDEWEB)

    Shaltout, Abdallah A., E-mail: shaltout_a@hotmail.com [Spectroscopy Department, Physics Division, National Research Center, El Behooth Str., 12622 Dokki, Cairo (Egypt); Faculty of science, Taif University, 21974 Taif, P.O. Box 888 (Saudi Arabia); Moharram, Mohammed A. [Spectroscopy Department, Physics Division, National Research Center, El Behooth Str., 12622 Dokki, Cairo (Egypt); Mostafa, Nasser Y. [Faculty of science, Taif University, 21974 Taif, P.O. Box 888 (Saudi Arabia); Chemistry Department, Faculty of Science, Suez Canal University, Ismailia (Egypt)

    2012-01-15

    This work is the first attempt to quantify trace elements in the Catha edulis plant (Khat) with a fundamental parameter approach. C. edulis is a famous drug plant in east Africa and Arabian Peninsula. We have previously confirmed that hydroxyapatite represents one of the main inorganic compounds in the leaves and stalks of C. edulis. Comparable plant leaves from basil, mint and green tea were included in the present investigation as well as trifolium leaves were included as a non-related plant. The elemental analyses of the plants were done by Wavelength Dispersive X-Ray Fluorescence (WDXRF) spectroscopy. Standard-less quantitative WDXRF analysis was carried out based on the fundamental parameter approaches. According to the standard-less analysis algorithms, there is an essential need for an accurate determination of the amount of organic material in the sample. A new approach, based on the differential thermal analysis, was successfully used for the organic material determination. The obtained results based on this approach were in a good agreement with the commonly used methods. Depending on the developed method, quantitative analysis results of eighteen elements including; Al, Br, Ca, Cl, Cu, Fe, K, Na, Ni, Mg, Mn, P, Rb, S, Si, Sr, Ti and Zn were obtained for each plant. The results of the certified reference materials of green tea (NCSZC73014, China National Analysis Center for Iron and Steel, Beijing, China) confirmed the validity of the proposed method. - Highlights: Black-Right-Pointing-Pointer Quantitative analysis of Catha edulis was carried out using standardless WDXRF. Black-Right-Pointing-Pointer Differential thermal analysis was used for determination of the loss of ignition. Black-Right-Pointing-Pointer The existence of hydroxyapatite in Catha edulis plant has been confirmed. Black-Right-Pointing-Pointer The CRM results confirmed the validity of the developed method.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-12-15

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

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

    Science.gov (United States)

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

    2017-04-01

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

  10. Quantitative analysis of total reflection X-ray fluorescence from finely layered structures using XeRay

    Energy Technology Data Exchange (ETDEWEB)

    Gong, Zhiliang [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Kerr, Daniel [Program in the Biophysical Sciences, Institute for Biophysical Dynamics, The University of Chicago, Chicago, Illinois 60637, USA; Hwang, Hyeondo Luke [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Henderson, J. Michael [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Suwatthee, Tiffany [The College, The University of Chicago, Chicago, Illinois 60637, USA; Slaw, Benjamin R. [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Cao, Kathleen D. [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Lin, Binhua [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Center for Advanced Radiation Sources, The University of Chicago, Chicago, Illinois 60637, USA; Bu, Wei [Center for Advanced Radiation Sources, The University of Chicago, Chicago, Illinois 60637, USA; Lee, Ka Yee C. [James Franck Institute, The University of Chicago, Chicago, Illinois 60637, USA; Department of Chemistry, The University of Chicago, Chicago, Illinois 60637, USA; Center for Advanced Radiation Sources, The University of Chicago, Chicago, Illinois 60637, USA

    2017-03-01

    Total reflection x-ray fluorescence (TXRF) is a widely applicable experimental technique for studying chemical element distributions across finely layered structures at extremely high sensitivity. To promote and facilitate scientific discovery using TXRF, we developed a MATLAB-based software package with a graphical user interface, named XeRay, for quick, accurate, and intuitive data analysis. XeRay lets the user model any layered system, each layer with its independent chemical composition and thickness, and enables fine-tuned data fitting. The accuracy of XeRay has been tested in the analysis of TXRF data from both air/liquid interface and liquid/liquid interfacial studies and has been compared to literature results. In an air/liquid interface study, Ca2+ sequestration was measured at a Langmuir monolayer of 1-stearoyl-2-oleoyl-sn-glycero-3-phosphatidic acid (SOPA) on a buffer solution of 1 mM CaCl2 at pH 7.5. Data analysis with XeRay reveals that each 1 nm2 of interfacial area contains 2.38 ± 0.06 Ca2+ ions, which corresponds to a 1:1 ratio between SOPA headgroups and Ca2+ ions, consistent with several earlier reports. For the liquid/liquid interface study of Sr2+ enrichment at the dodecane/surfactant/water interface, analysis using XeRay gives a surface enrichment of Sr2+ at 68+6-568-5+6 Å2 per ion, consistent with the result published for the same dataset.

  11. Determination of copper in geological materials by X-ray fluorescence; Determinacion de cobre en materiales geologicos mediante fluorescencia de rayos X

    Energy Technology Data Exchange (ETDEWEB)

    Roca, M.; Bayon, A.

    1981-07-01

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

  12. Measurement of photon-induced Ksub(. cap alpha. 1) and Ksub(. beta. 1) x-ray fluorescence cross-sections for some elements with 73 <= Z <= 82

    Energy Technology Data Exchange (ETDEWEB)

    Saleh, N.S.; Al-Saleh, K.A.

    1987-01-01

    Ksub(..cap alpha..1) and Ksub(..beta..1) x-ray fluorescence cross sections have been calculated for 10 elements with 73 <= Z <82 at the excitation energy of 121.9 keV ..gamma..-ray from /sup 57/Co radionuclide. Measurements were also made for these cross-sections for six elements with 73 <= Z <=82 at the same excitation energy from /sup 57/Co radionuclide. A comparison between the experimentally measured and the theoretically calculated values shows that the experimental results agree fairly well with the theoretical values within the uncertainties of the measurements. To the best of our knowledge, photon-induced Ksub(..cap alpha..1) and Ksub(..beta..1) x-ray fluorescence cross-sections for these elements at this excitation energy are being reported for the first time.

  13. Direct analysis of blood serum by total reflection X-ray fluorescence spectrometry and application of an artificial neural network approach for cancer diagnosis*1

    Science.gov (United States)

    Hernández-Caraballo, Edwin A.; Marcó-Parra, Lué M.

    2003-12-01

    Iron, copper, zinc and selenium were determined directly in serum samples from healthy individuals ( n=33) and cancer patients ( n=27) by total reflection X-ray fluorescence spectrometry using the Compton peak as internal standard [L.M. Marcó P. et al., Spectrochim. Acta Part B 54 (1999) 1469-1480]. The standardized concentrations of these elements were used as input data for two-layer artificial neural networks trained with the generalized delta rule in order to classify such individuals according to their health status. Various artificial neural networks, comprising a linear function in the input layer, a hyperbolic tangent function in the hidden layer and a sigmoid function in the output layer, were evaluated for such a purpose. Of the networks studied, the (4:4:1) gave the highest estimation (98%) and prediction rates (94%). The latter demonstrates the potential of the total reflection X-ray fluorescence spectrometry/artificial neural network approach in clinical chemistry.

  14. Energy dispersive X-ray fluorescence analysis of ancient coins: The case of Greek silver drachmae from the Emporion site in Spain

    Energy Technology Data Exchange (ETDEWEB)

    Pitarch, A., E-mail: apitarch@ija.csic.e [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' -ICTJA, Spanish Council for Scientific Research - CSIC, Lluis Sole Sabaris s/n, 08028 Barcelona (Spain); Queralt, I. [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' -ICTJA, Spanish Council for Scientific Research - CSIC, Lluis Sole Sabaris s/n, 08028 Barcelona (Spain)

    2010-05-15

    Greek colonizers arrived at the Iberian Peninsula at the beginning of the sixth century B.C. and founded a small colony known as Emporion in north-east Spain. By the fifth century B.C., this colony became a small polis with a well-organized administrative structure. In this context, the necessity of coinage was a fact and the first coins were minted. Some of these coins were characterized by using energy dispersive X-ray fluorescence equipment. The analytical study focused on the elemental characterization of the coins minted from the fourth century to the first century B.C. and their compositional evolution during this period. The investigation has pointed out a very high fineness of the alloys throughout the time, with an average silver content around 98.32%, and the feasibility of energy dispersive X-ray fluorescence as a screening tool for the characterization of the alloys.

  15. Phytopathology study through the X-ray fluorescence technique by energy dispersion; Estudo de fitopatologias atraves da tecnica de fluorescencia de raios X por dispersao em energia

    Energy Technology Data Exchange (ETDEWEB)

    Aragao, Pedro Henrique Arruda; Mauro, Eduardo Di; Suguihiro, Natasha Midori [Universidade Estadual de Londrina, PR (Brazil). Dept. de Fisica]. E-mail: phtd@uel.br; Rampazo, Luis Gustavo de Lazaro [Universidade Estadual de Londrina, PR (Brazil). Dept. de Microbiologia; Melo, Mauricio Antonio C de; Paesano Junior, Andrea [Universidade Estadual de Maringa, PR (Brazil). Dept. de Fisica; Nascimento Filho, Virgilio do Franco [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Metodologia de Radioisotopos

    2002-07-01

    In this paper energy dispersive X-ray fluorescence has been used to study two phytopathology 'sooty moulds' and 'citrus cancro' in olive trees, orange trees, lemon trees, etc. Energy dispersive X-ray fluorescence was used to analyse leaves samples of these trees. We have studied samples including leaves with and without infection by sooty moulds and citrus cancro. A correlation among elements of Fe and Ca has been observed. In the case of infected leaves a significant increasing in Fe concentration and decreasing in Ca concentration has been detected. This correlation is a pattern of all methods using in the paper. The high concentration of Fe in the infected leaves makes use the EPR and Moessbauer spectroscopes. We determined and concluded that the state of oxidation of the Fe is the Fe{sup +3}. (author)

  16. Energy dispersive X-ray fluorescence analysis of ancient coins: The case of Greek silver drachmae from the Emporion site in Spain

    Science.gov (United States)

    Pitarch, A.; Queralt, I.

    2010-05-01

    Greek colonizers arrived at the Iberian Peninsula at the beginning of the sixth century B.C. and founded a small colony known as Emporion in north-east Spain. By the fifth century B.C., this colony became a small polis with a well-organized administrative structure. In this context, the necessity of coinage was a fact and the first coins were minted [1]. Some of these coins were characterized by using energy dispersive X-ray fluorescence equipment. The analytical study focused on the elemental characterization of the coins minted from the fourth century to the first century B.C. and their compositional evolution during this period. The investigation has pointed out a very high fineness of the alloys throughout the time, with an average silver content around 98.32%, and the feasibility of energy dispersive X-ray fluorescence as a screening tool for the characterization of the alloys.

  17. Suzaku Observation of Strong Fluorescent Iron Line Emission from the Young Stellar Object V1647 Ori during Its New X-ray Outburst

    Science.gov (United States)

    Hamaguchi, Kenji; Grosso, Nicolas; Kastner, Joel H.; Weintraub, David A.; Richmond, Michael

    2009-01-01

    The Suzaku X-ray satellite observed the young stellar object V1647 Ori on 2008 October 8 during the new mass accretion outburst reported in August 2008. During the 87 ksec observation with a net exposure of 40 ks, V1647 Ori showed a. high level of X-ray emission with a gradual decrease in flux by a factor of 5 and then displayed an abrupt flux increase by an order of magnitude. Such enhanced X-ray variability was also seen in XMM-Newton observations in 2004 and 2005 during the 2003-2005 outburst, but has rarely been observed for other young stellar objects. The spectrum clearly displays emission from Helium-like iron, which is a signature of hot plasma (kT approx.5 keV). It also shows a fluorescent iron Ka line with a remarkably large equivalent width of approx. 600 eV. Such a, large equivalent width indicates that a part of the incident X-ray emission that irradiates the circumstellar material and/or the stellar surface is hidden from our line of sight. XMM-Newton spectra during the 2003-2005 outburst did not show a strong fluorescent iron Ka line ; so that the structure of the circumstellar gas very close to the stellar core that absorbs and re-emits X-ray emission from the central object may have changed in between 2005 and 2008. This phenomenon may be related to changes in the infrared morphology of McNeil's nebula between 2004 and 2008.

  18. A simple X-ray emitter.

    Science.gov (United States)

    Murakami, Hiroaki; Ono, Ryoichi; Hirai, Atsuhiko; Hosokawa, Yoshinori; Kawai, Jun

    2005-07-01

    A compact X-ray emission instrument is made, and the X-ray spectra are measured by changing the applied electric potential. Strong soft X-rays are observed when evacuating roughly and applying a high voltage to an insulator settled in this device. The X-ray intensity is higher as the applied voltage is increased. A light-emitting phenomenon is observed when this device emits X-rays. The present X-ray emitter is made of a small cylinder with a radius of 20 mm and a height of 50 mm. This X-ray generator has a potential to be used as an X-ray source in an X-ray fluorescence spectrometer.

  19. Bias correction by use of errors-in-variables regression models in studies with K-X ray fluorescence bone lead measurements1

    OpenAIRE

    Lamadrid-Figueroa, Héctor; Téllez-Rojo, Martha M.; Ángeles, Gustavo; Hernández-Ávila, Mauricio; Hu, Howard

    2010-01-01

    In-vivo measurement of bone lead by means of K-X ray fluorescence (KXRF) is the preferred biological marker of chronic exposure to lead. Unfortunately, considerable measurement error associated with KXRF estimations can introduce bias in estimates of the effect of bone lead when this variable is included as the exposure in a regression model. Estimates of uncertainty reported by the KXRF instrument reflect the variance of the measurement error and, although they can be used to correct the mea...

  20. Addition of X-ray fluorescent tracers into polymers, new technology for automatic sorting of plastics : proposal for selecting some relevant tracers

    OpenAIRE

    BEZATI, Feliks; FROELICH, Daniel; Massardier,Valérie; Maris, Elisabeth

    2011-01-01

    A description of a new technology for automatic sorting of plastics, based on X-ray fluorescence detection of tracers, added in such materials is presented. This study describes the criteria for the selection of tracers, and concluded that the most adapted for XRF are some rare earth oxides. The plastics chosen for tracing and identification are the ones contained in ELV and WEEE from which discrimination is difficult for the existing sorting techniques due to their black colour.; A descripti...

  1. The interaction between atoms of Au and Cu with clean Si(111) surface: a study combining synchrotron radiation grazing incidence X-ray fluorescence analysis and theoretical calculations.

    Science.gov (United States)

    de Carvalho, Hudson W P; Batista, Ana P L; Ramalho, Teodorico C; Pérez, Carlos A; Gobbi, Angelo Luiz

    2009-09-15

    In order to evaluate the interactions between Au/Cu atoms and clean Si(111) surface, we used synchrotron radiation grazing incidence X-ray fluorescence analysis and theoretical calculations. Optimized geometries and energies on different adsorption sites indicate that the binding energies at different adsorption sites are high, suggesting a strong interaction between metal atom and silicon surface. The Au atom showed higher interaction than Cu atom. The theoretical and experimental data showed good agreement.

  2. Refracted x-ray fluorescence (RXF) applied to the study of thermally grown oxide scales on Fe-Cr-Ni-(RE) alloys.

    Energy Technology Data Exchange (ETDEWEB)

    Koshelev, I.

    1998-06-03

    Refracted X-Ray Fluorescence (RXF) is applied to the study of the thermally grown scales on Fe25Cr20Ni(RE) alloys. The evolution of chromia scales is investigated for alloys containing reactive elements (RE) Y and Zr as well as the corresponding RE-free alloy. For these alloys, scale compositions, scale thicknesses and growth rates are measured and information about concentration depth profiles is obtained.

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

    OpenAIRE

    Watanabe, Yoshihide; Nishimura, Yusaku F.; Suzuki, Ryo; Uehara, Hiromitsu; Nimura, Tomoyuki; Beniya, Atsushi; Isomura, Noritake; Asakura, Kiyotaka; Takakusagi, Satoru

    2016-01-01

    A portable ultrahigh-vacuum sample storage system was designed and built to investigate the detailed geometric structures of mass-selected metal clusters on oxide substrates by polarization-dependent total-reflection fluorescence x-ray absorption fine structure spectroscopy (PTRF-XAFS). This ultrahigh-vacuum (UHV) sample storage system provides the handover of samples between two different sample manipulating systems. The sample storage system is adaptable for public transportation, facilitat...

  4. Origin of magnetic circular dichroism in soft x-ray fluorescence of Heusler alloys at threshold excitation

    Energy Technology Data Exchange (ETDEWEB)

    Yablonskikh, M. V.; Yarmoshenko, Yu. M.; Grebennikov, V. I.; Kurmaev, E. Z.; Butorin, S. M.; Duda, L.-C.; Nordgren, J.; Plogmann, S.; Neumann, M.

    2001-06-15

    The results of investigations of the Heusler alloys NiMnSb and Co{sub 2}MnSb by magnetic circular dichroism in soft x-ray emission spectroscopy (SXEMCD) are presented. The data obtained are in a good agreement with theoretical calculations of x-ray emission. A very intense resonant inelastic peak in the Mn L{sub 3} spectra in the region of states above the nominal Fermi level was observed and attributed to x-ray reemission. The interplay between the theoretically predicted half-metallic character of the Mn 3d valence band and the Mn L{sub 2},L{sub 3} SXEMCD spectra is discussed.

  5. Characterization of the External and Internal Flow Structure of an Aerated-Liquid Injector using X-Ray Radiography and Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Peltier, Scott J.; Lin, Kuo-Cheng; Carter, Campbell D.; Kastengren, Alan L.

    2017-09-01

    In the present study, the internal flowfield of aerated-liquid fuel injectors is examined through x-ray radiography and x-ray fluorescence. An inside-out injector, consisting of a perforated aerating tube within an annular liquid stream, sprays into a quiescent environment at a fixed mass flow rate of water and nitrogen gas. The liquid is doped with bromine (in the form of NaBr) to create an x-ray fluorescence signal. This allows for reasonable absorption and fluorescence signals, and one or both diagnostics can be used to track the liquid distribution. The injector housing is fabricated from beryllium (Be), which allows the internal flowfield to be examined (as Be has relatively low x-ray attenuation coefficient). Two injector geometries are compared, illustrating the effects of aerating orifice size and location on the flow evolution. Time-averaged equivalent pathlength (EPL) and line-of-sight averaged density ρ(y) reveal the formation of the two-phase mixture, showing that the liquid film thickness along the injector walls is a function of the aerating tube geometry, though only upstream of the nozzle. These differences in gas and liquid distribution (between injectors with different aerating tube designs) are suppressed as the mixture traverses the nozzle contraction. The averaged liquid velocity (computed from the density and liquid mass flow rate) reveal a similar trend. This suggests that at least for the current configurations, the plume width, liquid mass distribution, and averaged liquid velocity for the time-averaged external spray are insensitive to the aerating tube geometry.

  6. Characterization of the external and internal flow structure of an aerated-liquid injector using X-ray radiography and fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Peltier, Scott J. [Aerospace Systems Directorate, Air Force Research Laboratory, Arnold AFB, TN (United States); Lin, Kuo-Cheng [Taitech, Inc., Beavercreek, OH (United States); Carter, Campbell D. [Aerospace Systems Directorate, Air Force Research Laboratory, Wright-Patterson AFB, OH (United States); Kastengren, Alan L. [Argonne National Laboratory, X-Ray Science Division, Advanced Photon Source, Argonne, IL (United States)

    2017-09-15

    In the present study, the internal flowfield of aerated-liquid fuel injectors is examined through X-ray radiography and X-ray fluorescence. An inside-out injector, consisting of a perforated aerating tube within an annular liquid stream, sprays into a quiescent environment at a fixed mass flow rate of water and nitrogen gas. The liquid is doped with bromine (in the form of NaBr) to create an X-ray fluorescence signal. This allows for reasonable absorption and fluorescence signals, and one or both diagnostics can be used to track the liquid distribution. The injector housing is fabricated from beryllium (Be), which allows the internal flowfield to be examined (as Be has relatively low X-ray attenuation coefficient). Two injector geometries are compared, illustrating the effects of aerating orifice size and location on the flow evolution. Time-averaged equivalent pathlength and line-of-sight averaged density ρ(y) reveal the formation of the two-phase mixture, showing that the liquid film thickness along the injector walls is a function of the aerating tube geometry, though only upstream of the nozzle. These differences in gas and liquid distribution (between injectors with different aerating tube designs) are suppressed as the mixture traverses the nozzle contraction. The averaged liquid velocity (computed from the density and liquid mass flow rate) reveals a similar trend. This suggests that at least for the current configurations, the plume width, liquid mass distribution, and averaged liquid velocity for the time-averaged external spray are insensitive to the aerating tube geometry. (orig.)

  7. The weak Fe fluorescence line and long-term X-ray evolution of the Compton-thick active galactic nucleus in NGC 7674

    Science.gov (United States)

    Gandhi, P.; Annuar, A.; Lansbury, G. B.; Stern, D.; Alexander, D. M.; Bauer, F. E.; Bianchi, S.; Boggs, S. E.; Boorman, P. G.; Brandt, W. N.; Brightman, M.; Christensen, F. E.; Comastri, A.; Craig, W. W.; Del Moro, A.; Elvis, M.; Guainazzi, M.; Hailey, C. J.; Harrison, F. A.; Koss, M.; Lamperti, I.; Malaguti, G.; Masini, A.; Matt, G.; Puccetti, S.; Ricci, C.; Rivers, E.; Walton, D. J.; Zhang, W. W.

    2017-06-01

    We present NuSTAR X-ray observations of the active galactic nucleus (AGN) in NGC 7674. The source shows a flat X-ray spectrum, suggesting that it is obscured by Compton-thick gas columns. Based upon long-term flux dimming, previous work suggested the alternate possibility that the source is a recently switched-off AGN with the observed X-rays being the lagged echo from the torus. Our high-quality data show the source to be reflection-dominated in hard X-rays, but with a relatively weak neutral Fe Kα emission line (equivalent width [EW] of ≈ 0.4 keV) and a strong Fe xxvi ionized line (EW ≈ 0.2 keV). We construct an updated long-term X-ray light curve of NGC 7674 and find that the observed 2-10 keV flux has remained constant for the past ≈ 20 yr, following a high-flux state probed by Ginga. Light travel time arguments constrain the minimum radius of the reflector to be ˜ 3.2 pc under the switched-off AGN scenario, ≈ 30 times larger than the expected dust sublimation radius, rendering this possibility unlikely. A patchy Compton-thick AGN (CTAGN) solution is plausible, requiring a minimum line-of-sight column density (NH) of 3 × 1024 cm-2 at present, and yields an intrinsic 2-10 keV luminosity of (3-5) × 1043 erg s-1. Realistic uncertainties span the range of ≈ (1-13) × 1043 erg s-1. The source has one of the weakest fluorescence lines amongst bona fide CTAGN, and is potentially a local analogue of bolometrically luminous systems showing complex neutral and ionized Fe emission. It exemplifies the difficulty of identification and proper characterization of distant CTAGN based on the strength of the neutral Fe Kα line.

  8. A rapid total reflection X-ray fluorescence protocol for micro analyses of ion profiles in Arabidopsis thaliana

    Science.gov (United States)

    Höhner, Ricarda; Tabatabaei, Samaneh; Kunz, Hans-Henning; Fittschen, Ursula

    2016-11-01

    The ion homeostasis of macro and micronutrients in plant cells and tissues is a fundamental requirement for vital biochemical pathways including photosynthesis. In nature, ion homeostasis is affected mainly by three processes: 1. Environmental stress factors, 2. Developmental effects, and 3. Loss or gain-of-function mutations in the plant genome. Here we present a rapid total reflection X-ray fluorescence (TXRF) protocol that allows for simultaneous quantification of several elements such as potassium (K), calcium (Ca), sulfur (S), manganese (Mn) and strontium (Sr) in Arabidopsis thaliana leaf specimens. Our procedure is cost-efficient and enables precise, robust and highly reproducible measurements on tissue samples as small as 0.3 mg dry weight. As shown here, we apply the TXRF procedure to detect accurately the early replacement of K by Na ions in leaves of plants exposed to soil salinity, a globally increasing abiotic stress factor. Furthermore, we were able to prove the existence of a leaf development-dependent ion gradient for K, Ca, and other divalent ions in A. thaliana; i.e. old leaves contain significantly lower K but higher Ca than young leaves. Lastly, we show that our procedure can be readily applied to reveal subtle differences in tissue-specific ion contents of plant mutants. We employed independent A. thaliana kea1kea2 loss-of-function mutants that lack KEA1 and KEA2, two highly active chloroplast K exchange proteins. We found significantly increased K levels specifically in kea1kea2 mutants, i.e. 55 mg ∗ g- 1 dry weight, compared to 40 mg ∗ g- 1 dry weight in wild type plants. The TXRF procedure can be supplemented with Flame atomic absorption (FAAS) and emission spectrometry (FAES) to expand the detection range to sodium (Na) and magnesium (Mg). Because of the small sample amounts required, this method is especially suited to probe individual leaves in single plants or even specific leaf areas. Therefore, TXRF represents a powerful method to

  9. Evaluation of X-ray fluorescence spectroscopy as a method for the rapid and direct determination of sodium in cheese.

    Science.gov (United States)

    Stankey, J A; Akbulut, C; Romero, J E; Govindasamy-Lucey, S

    2015-08-01

    Cheese manufacturers indirectly determine Na in cheese by analysis of Cl using the Volhard method, assuming that all Cl came from NaCl. This method overestimates the actual Na content in cheeses when Na replacers (e.g., KCl) are used. A direct and rapid method for Na detection is needed. X-ray fluorescence spectroscopy (XRF), a mineral analysis technique used in the mining industry, was investigated as an alternative method of Na detection in cheese. An XRF method for the detection of Na in cheese was developed and compared with inductively coupled plasma optical emission spectroscopy (ICP-OES; the reference method for Na in cheese) and Cl analyzer. Sodium quantification was performed by multi-point calibration with cheese standards spiked with NaCl ranging from 0 to 4% Na (wt/wt). The Na concentration of each of the cheese standards (discs: 30mm×7mm) was quantified by the 3 methods. A single laboratory method validation was performed; linearity, precision, limit of detection, and limit of quantification were determined. An additional calibration graph was created using cheese standards made from natural or process cheeses manufactured with different ratios of Na:K. Both Na and K calibration curves were linear for the cheese standards. Sodium was quantified in a variety of commercial cheese samples. The Na data obtained by XRF were in agreement with those from ICP-OES and Cl analyzer for most commercial natural cheeses. The XRF method did not accurately determine Na concentration for several process cheese samples, compared with ICP-OES, likely due to the use of unknown types of Na-based emulsifying salts (ES). When a calibration curve was created for process cheese with the specific types of ES used for this cheese, Na content was successfully predicted in the samples. For natural cheeses, the limit of detection and limit of quantification for Na that can be determined with an acceptable level of repeatability, precision, and trueness was 82 and 246mg/100g of

  10. Sulfur L{sub 2,3} soft-x-ray fluorescence of CdS and ZnS

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, L.; Callcott, T.A.; Jia, J.J. [Univ. of Tennessee, Knoxville, TN (United States)] [and others

    1997-04-01

    The II-VI sulfur compounds CdS and ZnS have important electro-optics applications. In addition, they have well characterized and relatively simple structures so that they are good candidates for theoretical model development in solid-state physics. Some experimental results on density of states have been reported, mostly determined from photoemission measurements, and theoretical calculations are available for both materials. Nevertheless the electronic properties of these elements are still not completely understood. It has been established that the d-bands, derived from Cd or Zn, lie in a subband gap between a lower valence band (LVB) derived from the S 3s orbital and an upper valence band (UVB) derived from the 3p states of S and the 4(3)s states of Cd(Zn). The locations of these bands within the gap disagree with the best available calculations, however. The principal problem is that experimental photoemission measurements locate the d-bands about 2 eV lower in the band gap than the best available calculations. Some authors argue that the hole in the d-band in the final state of the photoemission process increases the binding of the d-electrons. In any case, band gaps, band widths and the precise location of d-bands are important parameters for comparing experiment and theory, and no current calculations give good agreement with all of these parameters. Moreover, photoemission data does not adequately define all of these experimental parameters, because the d-state photoemission dominates that from s and p states and sample charging effects can modify the energy of emitted electrons. The authors report photon excited soft x-ray fluorescence (SXF) S L{sub 2,3} spectra from CdS and ZnS. Using excitation between the L{sub 2} and L{sub 3} thresholds, the L{sub 2} spectrum is suppressed, which permits the authors to accurately determine features of the UVB and LVB as well as the placement of the Cd(Zn) d-bands between the UVB and LVB.

  11. Surface and in-depth characterization of lithium-ion battery cathodes at different cycle states using confocal micro-X-ray fluorescence-X-ray absorption near edge structure analysis

    Energy Technology Data Exchange (ETDEWEB)

    Menzel, Magnus; Schlifke, Annalena [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Falk, Mareike; Janek, Jürgen [Physikalisch-Chemisches Institut, Justus-Liebig-Universität Gießen, Heinrich-Buff-Ring 58, 35392 Gießen (Germany); Fröba, Michael, E-mail: froeba@chemie.uni-hamburg.de [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany); Fittschen, Ursula Elisabeth Adriane, E-mail: ursula.fittschen@chemie.uni-hamburg.de [Institut für Anorganische und Angewandte Chemie, Universität Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany)

    2013-07-01

    The cathode material LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} for lithium-ion batteries has been studied with confocal micro-X-ray fluorescence (CMXRF) combined with X-ray absorption near edge structure (XANES) at the Mn-K edge and the Ni-K edge. This technique allows for a non-destructive, spatially resolved (x, y and z) investigation of the oxidation states of surface areas and to some extent of deeper layers of the electrode. Until now CMXRF-XANES has been applied to a limited number of applications, mainly geo-science. Here, we introduce this technique to material science applications and show its performance to study a part of a working system. A novel mesoporous LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} material was cycled (charged and discharged) to investigate the effects on the oxidation states at the cathode/electrolyte interface. With this approach the degradation of Mn{sup 3+} to Mn{sup 4+} only observable at the surface of the electrode could be directly shown. The spatially resolved non-destructive analysis provides knowledge helpful for further understanding of deterioration and the development of high voltage battery materials, because of its nondestructive nature it will be also suitable to monitor processes during battery cycling. - Highlights: • The potential of confocal micro-XRF-XANES for spatial resolved species analysis in a part of a working system is shown. • The spatial resolution enables differentiation of the oxidized interface from deeper layers. • With the analytical technique confocal micro-XRF-XANES 3D in-situ analyses of working systems are feasible. • The multidimensional and nondestructive analysis of Li-ion battery cathodes is shown. • The analysis will allow for a deeper understanding of processes at interfaces in battery science and others.

  12. Practical review on the use of synchrotron based micro- and nano- X-ray fluorescence mapping and X-ray absorption spectroscopy to investigate the interactions between plants and engineered nanomaterials.

    Science.gov (United States)

    Castillo-Michel, Hiram A; Larue, Camille; Pradas Del Real, Ana E; Cotte, Marine; Sarret, Geraldine

    2017-01-01

    The increased use of engineered nanomaterials (ENMs) in commercial products and the continuous development of novel applications, is leading to increased intentional and unintentional release of ENMs into the environment with potential negative impacts. Particularly, the partition of nanoparticles (NPs) to waste water treatment plant (WWTP) sludge represents a potential threat to agricultural ecosystems where these biosolids are being applied as fertilizers. Moreover, several applications of ENMs in agriculture and soil remediation are suggested. Therefore, detailed risk assessment should be done to evaluate possible secondary negative impacts. The impact of ENMS on plants as central component of ecosystems and worldwide food supply is of primary relevance. Understanding the fate and physical and chemical modifications of NPs in plants and their possible transfer into food chains requires specialized analytical techniques. Due to the importance of both chemical and physical factors to consider for a better understanding of ENMs behavior in complex matrices, these materials can be considered a new type of analyte. An ideal technique should require minimal sample preparation, be non-destructive, and offer the best balance between sensitivity, chemical specificity, and spatial resolution. Synchrotron radiation (SR) techniques are particularly adapted to investigate localization and speciation of ENMs in plants. SR X-ray fluorescence mapping (SR-XFM) offers multi-elemental detection with lateral resolution down to the tens of nm, in combination with spatially resolved X-ray absorption spectroscopy (XAS) speciation. This review will focus on important methodological aspects regarding sample preparation, data acquisition and data analysis of SR-XFM/XAS to investigate interactions between plants and ENMs. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  13. Rapid and non-destructive analysis of metallic dental restorations using X-ray fluorescence spectra and light-element sampling tools

    Science.gov (United States)

    Furuhashi, K.; Uo, M.; Kitagawa, Y.; Watari, F.

    2012-12-01

    IntroductionRecently, allergic diseases caused by dental metals have been increasing. Therefore, rapid and accurate analytical methods for the metal restorations in the oral cavities of patients are required. The purpose of this study was to develop a non-destructive extraction method for dental alloys, along with a subsequent, rapid and accurate elemental analysis. Materials and methodSamples were obtained by polishing the surfaces of metal restorations using a dental rotating tool with disposable buffs and polishing pastes. As materials for the analysis, three dental alloys were used. To compare the sampling and analysis efficiencies, two buffs and seven pastes were used. After polishing the surface of a metal restoration, the buff was analyzed using X-ray scanning analytical microscopy (XSAM). ResultsThe efficiency of the analysis was judged based on the sampling rate achieved and the absence of disturbing elements in the background in fluorescence X-ray spectra. The best results were obtained for the combination of TexMet as a buff with diamond as a paste. This combination produced a good collection efficiency and a plain background in the fluorescence X-ray spectra, resulting in a high precision of the analysis.

  14. Elements in normal and cirrhotic human liver. Potassium, iron, copper, zinc and bromine measured by X-ray fluorescence spectrometry

    DEFF Research Database (Denmark)

    Laursen, J.; Milman, N.; Leth, Peter Mygind

    1990-01-01

    Various elements (K, Fe, Cu, Zn, Br) were measured by X-ray flourescence spectrometry in cellular and connective tissue fractions of normal and cirrhotic liver samples obtained at autopsy. Normal livers: 32 subjects (16 males, 16 females) median age 69 years. Cirrhotic livers: 14 subjects (13 males...

  15. Confocal depth-resolved fluorescence micro-X-ray absorption spectroscopy for the study of cultural heritage materials: a new mobile endstation at the Beijing Synchrotron Radiation Facility.

    Science.gov (United States)

    Chen, Guang; Chu, Shengqi; Sun, Tianxi; Sun, Xuepeng; Zheng, Lirong; An, Pengfei; Zhu, Jian; Wu, Shurong; Du, Yonghua; Zhang, Jing

    2017-09-01

    A confocal fluorescence endstation for depth-resolved micro-X-ray absorption spectroscopy is described. A polycapillary half-lens defines the incident beam path and a second polycapillary half-lens at 90° defines the probe sample volume. An automatic alignment program based on an evolutionary algorithm is employed to make the alignment procedure efficient. This depth-resolved system was examined on a general X-ray absorption spectroscopy (XAS) beamline at the Beijing Synchrotron Radiation Facility. Sacrificial red glaze (AD 1368-1644) china was studied to show the capability of the instrument. As a mobile endstation to be applied on multiple beamlines, the confocal system can improve the function and flexibility of general XAS beamlines, and extend their capabilities to a wider user community.

  16. Confocal depth-resolved fluorescence micro-X-ray absorption spectroscopy for the study of cultural heritage materials: a new mobile endstation at the Beijing Synchrotron Radiation Facility

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Guang; Chu, Shengqi; Sun, Tianxi; Sun, Xuepeng; Zheng, Lirong; An, Pengfei; Zhu, Jian; Wu, Shurong; Du, Yonghua; Zhang, Jing

    2017-08-10

    A confocal fluorescence endstation for depth-resolved micro-X-ray absorption spectroscopy is described. A polycapillary half-lens defines the incident beam path and a second polycapillary half-lens at 90° defines the probe sample volume. An automatic alignment program based on an evolutionary algorithm is employed to make the alignment procedure efficient. This depth-resolved system was examined on a general X-ray absorption spectroscopy (XAS) beamline at the Beijing Synchrotron Radiation Facility. Sacrificial red glaze (AD 1368–1644) china was studied to show the capability of the instrument. As a mobile endstation to be applied on multiple beamlines, the confocal system can improve the function and flexibility of general XAS beamlines, and extend their capabilities to a wider user community.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  18. In situ characterization of ancient plaster and pigments on tomb walls in Egypt using energy dispersive X-ray diffraction and fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Uda, M. E-mail: muda@waseda.jp

    2004-11-01

    A portable type of energy dispersive X-ray diffraction and fluorescence (ED-XRDF) spectrometer was developed, whose operation mode is completely different from that of an X-ray diffractometer commercially available. The former is operated in energy dispersive mode but the latter in angle dispersive mode. The performance of the ED-XRDF spectrometer was tested in the field, i.e. in the tomb of Amenhotep III, built in 1364 B.C. or earlier in Egypt. The crystal structure and chemical composition of ancient plaster and pigments were successfully determined in the field using the spectrometer. The same areas investigated by the ED-XRDF spectrometer were also examined with an optical microscope. The plaster is found to be composed of anhydrite, calcite and quartz. White and yellow pigments were identified as huntite and orpiment, respectively. Egyptian blue and goethite were found in the green colored parts.

  19. Joint x-ray

    Science.gov (United States)

    X-ray - joint; Arthrography; Arthrogram ... x-ray technologist will help you position the joint to be x-rayed on the table. Once in place, pictures are taken. The joint may be moved into other positions for more ...

  20. Whole body in vivo examination of small animals by simultaneous X-rays/optical tomography: comparison between the reconstructions obtained with different types of fluorescent labels

    Science.gov (United States)

    Da Silva, A.; Bordy, T.; Debourdeau, M.; Dinten, J.-M.; Peltié, P.; Rizo, P.

    2007-07-01

    Small animal diffuse optical tomography is an appealing tool for the investigation of molecular events in cancer research and drug developments. The combination of the functional information brought by an optical system and the anatomical information delivered by X-Rays enables i) a fast multimodality animal examination; ii) the correlation between the biodistribution of the molecular probes and the morphology of the animal; iii) a more accurate optical data reconstructions by using the anatomy of the animal as a constrain in the reconstructions. A small animal multimodality tomographer for the coregistration of fluorescence optical signals and X-rays measurements is used in the present study. The optical system is composed with a CW laser and a CCD camera coupled with an appropriate combination of filters for the fluorescence detection. The animal is placed inside a transparent tube filled with an index matching fluid. The X-ray generator and detector have been positioned perpendicularly to the optical chain. Original optical calibration techniques have been developed in order to control at any time the alignment between the incident beam, the axis of the cylinder and the focus plan of the CCD. Specific developments have also been handled for obtaining the geometry correlation between optical and X-rays data reconstructions. This experimental setup is used in the present work for a study conducted on different kinds of fluorochromes for the purpose of the development of new molecular probes. The instrument is also used for in vivo biological study conducted on mice bearing tumors in the lungs, and tagged with near infrared optical probes (targeting probes such as Transferin- AlexaFluor 750 or such as RAFT-(cRGD) 4-Alexa700/Alexa750).

  1. Correlation between Wavelength Dispersive X-ray Fluorescence (WDXRF) analysis of hardened concrete for chlorides vs. Atomic Absorption (AA) analysis in accordance with AASHTO T- 260; sampling and testing for chloride ion in concrete and concrete raw mater

    Science.gov (United States)

    2014-04-01

    A correlation between Wavelength Dispersive X-ray Fluorescence(WDXRF) analysis of Hardened : Concrete for Chlorides and Atomic Absorption (AA) analysis (current method AASHTO T-260, procedure B) has been : found and a new method of analysis has been ...

  2. Evaluation of a new X-ray fluorescent analysis technique for the creation of a Nordic hair database: elemental distributions within the root and the virgin segment of hair fibers

    National Research Council Canada - National Science Library

    Stocklassa, B; Aransay-Vitores, M; Nilsson, G; Karlsson, C; Wiegleb, D; Forslind, B

    2001-01-01

    .... Thus, attenuation variations of the fluorescent X-rays in the hair bulk mass were demonstrated by analysis of sulfur, calcium, and zinc in a virgin part near the root of one hair fiber with elliptical cross section...

  3. Study of a unique 16th century Antwerp majolica floor in the Rameyenhof castle's chapel by means of X-ray fluorescence and portable Raman analytical instrumentation

    Energy Technology Data Exchange (ETDEWEB)

    Van de Voorde, Lien, E-mail: lien.vandevoorde@ugent.be [Ghent University, Department of Analytical Chemistry, X-Ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Ghent (Belgium); Vandevijvere, Melissa [Ghent University, Department of Analytical Chemistry, X-Ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Ghent (Belgium); University of Antwerp, Faculty of Architecture and Design, Conservation Studies, Centre for Conservation Research (CCR), Blindestraat 9, 2000 Antwerp (Belgium); University of Antwerp, Department of Chemistry, X-ray and Instrumentation Lab (AXI2L), Groenenborgerlaan 171, 2020 Antwerp (Belgium); Vekemans, Bart [Ghent University, Department of Analytical Chemistry, X-Ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Ghent (Belgium); Van Pevenage, Jolien [Ghent University, Department of Analytical Chemistry, Raman Spectroscopy Research Group, Krijgslaan 281 S12, B-9000 Ghent (Belgium); Caen, Joost [University of Antwerp, Faculty of Architecture and Design, Conservation Studies, Centre for Conservation Research (CCR), Blindestraat 9, 2000 Antwerp (Belgium); Vandenabeele, Peter [Ghent University, Department of Archaeology, Archaeometry Research Group, Sint-Pietersnieuwstraat 35, B-9000 Ghent (Belgium); Van Espen, Piet [University of Antwerp, Department of Chemistry, X-ray and Instrumentation Lab (AXI2L), Groenenborgerlaan 171, 2020 Antwerp (Belgium); Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, X-Ray Microspectroscopy and Imaging Research Group, Krijgslaan 281 S12, B-9000 Ghent (Belgium)

    2014-12-01

    The most unique and only known 16th century Antwerp majolica tile floor in Belgium is situated in a tower of the Rameyenhof castle (Gestel, Belgium). This exceptional work of art has recently been investigated in situ by using X-ray fluorescence (XRF) and Raman spectroscopy in order to study the material characteristics. This study reports on the result of the analyses based on the novel combination of non-destructive and portable instrumentation, including a handheld XRF spectrometer for obtaining elemental information and a mobile Raman spectrometer for retrieving structural and molecular information on the floor tiles in the Rameyenhof castle and on a second, similar medallion, which is stored in the Rubens House museum in Antwerp (Belgium). The investigated material, majolica, is a type of ceramic, which fascinated many people and potters throughout history by its beauty and colourful appearance. In this study the characteristic major/minor and trace element signature of 16th century Antwerp majolica is determined and the pigments used for the colourful paintings present on the floor are identified. Furthermore, based on the elemental fingerprint of the white glaze, and in particular on the presence of zinc in the tiles – an element that was not used for making 16th century majolica – valuable information about the originality of the chapel floor and the two central medallions is acquired. - Highlights: • In situ, non-destructive investigation of a unique Antwerp majolica floor • Multi-methodological approach: make use of a mobile Raman and X-ray spectrometer • Obtaining information about layered structure of Antwerp majolica • The used pigments in the majolica floor in Rameyenhof castle are characterized. • The verification of the authenticity of the floor and two central medallions are performed.

  4. Visualisation of cell cycle modifications by X-ray irradiation of single HeLa cells using fluorescent ubiquitination-based cell cycle indicators.

    Science.gov (United States)

    Kaminaga, K; Noguchi, M; Narita, A; Sakamoto, Y; Kanari, Y; Yokoya, A

    2015-09-01

    To explore the effects of X-ray irradiation on mammalian cell cycle dynamics, single cells using the fluorescent ubiquitination-based cell cycle indicator (Fucci) technique were tracked. HeLa cells expressing Fucci were used to visualise cell cycle modifications induced by irradiation. After cultured HeLa-Fucci cells were exposed to 5 Gy X-rays, fluorescent cell images were captured every 20 min for 48 h using a fluorescent microscope. Time dependence of the fluorescence intensity of S/G2 cells was analysed to examine the cell cycle dynamics of irradiated and non-irradiated control cells. The results showed that irradiated cells could be divided into two populations: one with similar cell cycle dynamics to that of non-irradiated cells, and another displaying a prolonged G2 phase. Based on these findings, it is proposed in this article that an underlying switch mechanism is involved in cell cycle regulation and the G2/M checkpoint of HeLa cells. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  5. Semiconductor X-ray detectors

    CERN Document Server

    Lowe, Barrie Glyn

    2014-01-01

    Identifying and measuring the elemental x-rays released when materials are examined with particles (electrons, protons, alpha particles, etc.) or photons (x-rays and gamma rays) is still considered to be the primary analytical technique for routine and non-destructive materials analysis. The Lithium Drifted Silicon (Si(Li)) X-Ray Detector, with its good resolution and peak to background, pioneered this type of analysis on electron microscopes, x-ray fluorescence instruments, and radioactive source- and accelerator-based excitation systems. Although rapid progress in Silicon Drift Detectors (SDDs), Charge Coupled Devices (CCDs), and Compound Semiconductor Detectors, including renewed interest in alternative materials such as CdZnTe and diamond, has made the Si(Li) X-Ray Detector nearly obsolete, the device serves as a useful benchmark and still is used in special instances where its large, sensitive depth is essential. Semiconductor X-Ray Detectors focuses on the history and development of Si(Li) X-Ray Detect...

  6. Measurement of trace elements in KH/sub 2/PO/sub 4/ crystals by x-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ryon, R.W.; Duewer, T.I.

    1981-02-01

    A non-destructive method is described for the quantitative measurement of impurities in KDP (KH/sub 2/PO/sub 4/) crystals. Part per million concentrations of impurities can be determined with good accuracy in about one hour of instrument time. An energy dispersive x-ray spectrometer is used. Both the crystals and the solutions from which they are grown may be analyzed.

  7. X-ray spectrometry using polycapillary X-ray optics and position sensitive detector.

    Science.gov (United States)

    Ding, X; Xie, J; He, Y; Pan, Q; Yan, Y

    2000-10-02

    Polycapillary X-ray optics (capillary X-ray lens) are now popular in X-ray fluorescence (XRF) analysis. Such an X-ray lens can collect X-rays emitted from an X-ray source in a large solid angle and form a very intense X-ray microbeam which is very convenient for microbeam X-ray fluorescence (MXRF) analysis giving low minimum detection limits (MDLs) in energy dispersive X-ray fluorescence (EDXRF). A new method called position sensitive X-ray spectrometry (PSXS) which combines an X-ray lens used to form an intense XRF source and a position sensitive detector (PSD) used for wavelength dispersive spectrometry (WDS) measurement was developed recently in the X-ray Optics Laboratory of Institute of Low Energy Nuclear Physics (ILENP) at Beijing Normal University. Such a method can give high energy and spacial resolution and high detection efficiency simultaneously. A short view of development of both the EDXRF using a capillary X-ray lens and the new PSXS is given in this paper.

  8. Quantification of trace arsenic in soils by field-portable X-ray fluorescence spectrometry: considerations for sample preparation and measurement conditions.

    Science.gov (United States)

    Parsons, Chris; Margui Grabulosa, Eva; Pili, Eric; Floor, Geerke H; Roman-Ross, Gabriela; Charlet, Laurent

    2013-11-15

    Recent technological improvements have led to the widespread adoption of field portable energy dispersive X-ray fluorescence (FP-XRF) by governmental agencies, environmental consultancies and research institutions. FP-XRF units often include analysis modes specifically designed for the quantification of trace elements in soils. Using these modes, X-ray tube based FP-XRF units can offer almost "point and shoot" ease of use and results comparable to those of laboratory based instruments. Nevertheless, FP-XRF analysis is sensitive to spectral interferences as well as physical and chemical matrix effects which can result in decreased precision and accuracy. In this study, an X-ray tube-based FP-XRF analyser was used to determine trace (low ppm) concentrations of As in a floodplain soil. The effect of different sample preparation and analysis conditions on precision and accuracy were systematically evaluated. We propose strategies to minimise sources of error and maximise data precision and accuracy, achieving in situ limits of detection and precision of 6.8 ppm and 14.4%RSD, respectively for arsenic. We demonstrate that soil moisture, even in relatively dry soils, dramatically affects analytical performance with a signal loss of 37% recorded for arsenic at 20 wt% soil moisture relative to dry soil. We also highlight the importance of the use of certified reference materials and independent measurement methods to ensure accurate correction of field values. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Thermoelectrically cooled semiconductor detectors for non-destructive analysis of works of art by means of energy dispersive X-ray fluorescence

    CERN Document Server

    Cesareo, R; Castellano, A

    1999-01-01

    Thermoelectrically cooled semiconductor detectors, such as Si-PIN, Si-drift, Cd sub 1 sub - sub x Zn sub x Te and HgI sub 2 , coupled to miniaturized low-power X-ray tubes, are well suited in portable systems for energy-dispersive X-ray fluorescence (EDXRF), analysis of archaeological samples. The Si-PIN detector is characterized by a thickness of about 300 mu m, an area of about 2x3 mm sup 2 , an energy resolution of about 200-250 eV at 5.9 keV and an entrance window of 25-75 mu m. The Si-drift detector has approximately the same area and thickness, but an energy resolution of 155 eV at 5.9 keV. The efficiency of these detectors is around 100% from 4 to 10 keV, and then decreases versus energy, reaching approx 9% at 30 keV. Coupled to a miniaturized 10 kV, 0.1 mA, Ca-anode or to a miniaturized 30 kV, 0.1 mA, W-anode X-ray tubes, portable systems can be constructed, which are able to analyse K-lines of elements up to about silver, and L-lines of heavy elements. The Cd sub 1 sub - sub x Zn sub x Te detector ha...

  10. Imaging endosomes and autophagosomes in whole mammalian cells using correlative cryo-fluorescence and cryo-soft X-ray microscopy (cryo-CLXM)

    Energy Technology Data Exchange (ETDEWEB)

    Duke, Elizabeth M.H. [Diamond Light Source, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE (United Kingdom); Razi, Minoo [Secretory Pathways Laboratory, London Research Institute, Cancer Research UK, London WC2A 3LY (United Kingdom); Weston, Anne [Electron Microscopy Unit, London Research Institute, Cancer Research UK, London WC2A 3LY (United Kingdom); Guttmann, Peter; Werner, Stephan; Henzler, Katja; Schneider, Gerd [Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Institute for Soft Matter and Functional Materials, 12489 Berlin (Germany); Tooze, Sharon A. [Secretory Pathways Laboratory, London Research Institute, Cancer Research UK, London WC2A 3LY (United Kingdom); Collinson, Lucy M., E-mail: lucy.collinson@cancer.org.uk [Electron Microscopy Unit, London Research Institute, Cancer Research UK, London WC2A 3LY (United Kingdom)

    2014-08-01

    Cryo-soft X-ray tomography (cryo-SXT) is a powerful imaging technique that can extract ultrastructural information from whole, unstained mammalian cells as close to the living state as possible. Subcellular organelles including the nucleus, the Golgi apparatus and mitochondria have been identified by morphology alone, due to the similarity in contrast to transmission electron micrographs. In this study, we used cryo-SXT to image endosomes and autophagosomes, organelles that are particularly susceptible to chemical fixation artefacts during sample preparation for electron microscopy. We used two approaches to identify these compartments. For early and recycling endosomes, which are accessible to externally-loaded markers, we used an anti-transferrin receptor antibody conjugated to 10 nm gold particles. For autophagosomes, which are not accessible to externally-applied markers, we developed a correlative cryo-fluorescence and cryo-SXT workflow (cryo-CLXM) to localise GFP-LC3 and RFP-Atg9. We used a stand-alone cryo-fluorescence stage in the home laboratory to localise the cloned fluorophores, followed by cryo-soft X-ray tomography at the synchrotron to analyse cellular ultrastructure. We mapped the 3D ultrastructure of the endocytic and autophagic structures, and discovered clusters of omegasomes arising from ‘hotspots’ on the ER. Thus, immunogold markers and cryo-CLXM can be used to analyse cellular processes that are inaccessible using other imaging modalities. - Highlights: • We image whole, unstained mammalian cells using cryo-soft X-ray tomography. • Endosomes are identified using a gold marker for the transferrin receptor. • A new workflow for correlative cryo-fluorescence and cryo-SXT is used to locate early autophagosomes. • Interactions between endosomes, endoplasmic reticulum and forming autophagosomes are mapped in 3D. • Multiple omegasomes are shown to form at ‘hotspots’ on the endoplasmic reticulum.

  11. Analysis of agricultural soils by using energy dispersive X-ray fluorescence; Analise de solos agricolas por fluorescencia de raios-X por dispersao de energia

    Energy Technology Data Exchange (ETDEWEB)

    Anjos, Marcelino Jose dos

    2000-03-01

    In this work, we describe an Energy Dispersive x-ray Fluorescence System with a x-ray tube excitation for trace analysis of environmental samples (soil). The system was used to analyze the contamination of metals in treated soils with doses of 10, 20 and 30 ton/ha of compound organic of urban garbage of the type Fertilurb and 10 ton/ha of aviary bed (manure of birds). Samples of roots and foliages of plant radishes cultivated in these soils were also analyzed. The soil samples were collected in five different depths of 0,5, 5-10, 10-20, 20-40 and 40-60 cm. The experimental set-up is composed by an OXFORD X-ray (30 kV, 50 {mu}A and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray spectrum tube is quasi-monochromatic by using of Ti filter. Samples were prepared in pellet form with superficial density in the range of 100 mg/cm{sup 2}. The fundamental parameter method was used in order to verify the elemental concentration. It was possible to determine the concentrations of thirteen elements: K, Ca, Ti, Mn, Fe, Cu, Zn, Br, Rb, Sr, Y, Zr and Pb in the treated soils with compounds organic. The results indicate that the values found for K, Ca, Rb, Sr, Zr and Pb are significantly above the upper confidence limits for the control soil ({alpha} = 0.05). There is a real different between these elements compared to their relationship in the control soils, ({alpha}=0,05). There is a real difference between these elements compared to their relationship in the control soils, confirming the influence of the organic compounds in the soil. (author)

  12. Feasibility of different cleaning methods for silver-copper alloys by X-ray fluorescence: Application to ancient Greek silver coins

    Science.gov (United States)

    Moreno-Suárez, A. I.; Ager, F. J.; Rodríquez-Segovia, C.; Gómez-Morón, A.; Chaves, F.; Scrivano, S.; Gómez-Tubío, B.; Pliego, R.; Respaldiza, M. A.

    2016-02-01

    Archeological pieces with high Ag concentrations often have a surface enrichment of Ag. Usually, researchers in this field do not agree on the causes of these enrichments, one of which could be the cleaning procedures. In this work, a set of 18 ancient Greek silver coins was selected to study the effects of different cleaning procedures in terms of producing a surface Ag enrichment. The aim of this study is to find and select the less aggressive one in terms of the lower modification of Ag concentrations and visual aspect. These coins were analyzed by X-ray fluorescence (XRF) before and after each cleaning procedure.

  13. Determination of low concentrations of thorium in geological materials by X-ray fluorescence; Determinacion de bajas concentraciones de torio en materiales geologicos mediante fluorescencia de rayos X

    Energy Technology Data Exchange (ETDEWEB)

    Roca, M.; Bayon, A.

    1981-07-01

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

  14. Fast and direct Na and K determination in table, marine, and low-sodium salts by X-ray fluorescence and chemometrics.

    Science.gov (United States)

    Da-Col, José A; Bueno, Maria I M S; Melquiades, Fábio L

    2015-03-11

    X-ray fluorescence (XRF) is a fast, low-cost, nondestructive, and truly multielement analytical technique. The objectives of this study are to quantify the amount of Na(+) and K(+) in samples of table salt (refined, marine, and light) and to compare three different methodologies of quantification using XRF. A fundamental parameter method revealed difficulties in quantifying accurately lighter elements (Z fast. Na(+) quantifications provided calibration errors lower than 16% and a correlation of 0.995. Of great concern was the observation of high Na(+) levels in low-sodium salts. The presented application may be performed in a fast and multielement fashion, in accordance with Green Chemistry specifications.