Development of a micro-X-ray fluorescence system based on polycapillary X-ray optics for non-destructive analysis of archaeological objects

NASA Astrophysics Data System (ADS)

Cheng, Lin; Ding, Xunliang; Liu, Zhiguo; Pan, Qiuli; Chu, Xuelian

2007-08-01

A new micro-X-ray fluorescence (micro-XRF) system based on rotating anode X-ray generator and polycapillary X-ray optics has been set up in XOL Lab, BNU, China, in order to be used for analysis of archaeological objects. The polycapillary X-ray optics used here can focus the primary X-ray beam down to tens of micrometers in diameter that allows for non-destructive and local analysis of sub-mm samples with minor/trace level sensitivity. The analytical characteristics and potential of this micro-XRF system in archaeological research are discussed. Some described uses of this instrument include studying Chinese ancient porcelain.

Pots, plates and provenance: sourcing Indian coarse wares from Mleiha using X-ray fluorescence (XRF) spectrometry analysis

NASA Astrophysics Data System (ADS)

Reddy, A.; Attaelmanan, A. G.; Mouton, M.

2012-07-01

The identification of more than 25% of the pottery sherds from the late PIR.D period (ca. 2nd - mid. 3rd c. AD) assemblage from the recently excavated building H at Mleiha as Indian is based on form and fabric, but using only visual assessment. Petrographic analysis of the fabrics can provide more precise indicators of the geographical origin of the wares. In this study, a total of 21 sherds from various key sites in Western India were compared with 7 different 'Indian' coarse-ware vessels sampled at Mleiha using X-ray fluorescence (XRF) spectrometry. The analyses were conducted on powdered samples collected from the core of each sherd. Each sample was irradiated for 1000 seconds using a 1.2 mm diameter X-ray beam. The resulting spectra were used for quantification of the X-ray intensity and elemental concentration. Levels of correlation in the elemental ratios of the sherds were statistically tested using an F-test as well as a Chi-test. Initial review of the XRF results indicates that the Maharashtra and Gujarat regions of India are probable source areas for at least two of the types of wares. Collection of additional samples from these areas and other regions of India, and further statistical analysis through methods such as Principal Component Analysis will help to isolate groups of wares from India and correlate them with types of vessels imported into the Oman peninsula in antiquity.

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

NASA Technical Reports Server (NTRS)

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

2016-01-01

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

Pinhole X-ray fluorescence imaging of gadolinium and gold nanoparticles using polychromatic X-rays: a Monte Carlo study

PubMed Central

Jung, Seongmoon; Sung, Wonmo; Ye, Sung-Joon

2017-01-01

This work aims to develop a Monte Carlo (MC) model for pinhole K-shell X-ray fluorescence (XRF) imaging of metal nanoparticles using polychromatic X-rays. The MC model consisted of two-dimensional (2D) position-sensitive detectors and fan-beam X-rays used to stimulate the emission of XRF photons from gadolinium (Gd) or gold (Au) nanoparticles. Four cylindrical columns containing different concentrations of nanoparticles ranging from 0.01% to 0.09% by weight (wt%) were placed in a 5 cm diameter cylindrical water phantom. The images of the columns had detectable contrast-to-noise ratios (CNRs) of 5.7 and 4.3 for 0.01 wt% Gd and for 0.03 wt% Au, respectively. Higher concentrations of nanoparticles yielded higher CNR. For 1×1011 incident particles, the radiation dose to the phantom was 19.9 mGy for 110 kVp X-rays (Gd imaging) and 26.1 mGy for 140 kVp X-rays (Au imaging). The MC model of a pinhole XRF can acquire direct 2D slice images of the object without image reconstruction. The MC model demonstrated that the pinhole XRF imaging system could be a potential bioimaging modality for nanomedicine. PMID:28860750

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT OXFORD X-MTE 3000TX XRF ANALYZER

EPA Science Inventory

The Elvatech, Ltd. ElvaX (ElvaX) x-ray fluorescence (XRF) analyzer distributed in the United States by Xcalibur XRF Services (Xcalibur), was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field por...

Development of Standard Samples for on-board Calibration of a New Planetary X-Ray Fluorescence Spectrometer

NASA Astrophysics Data System (ADS)

Dreißigacker, Anne; Köhler, Eberhard; Fabel, Oliver; van Gasselt, Stephan

2014-05-01

At the Planetary Sciences and Remote Sensing research group at Freie Universität Berlin an SCD-based X-Ray Fluorescence Spectrometer is being developed to be employed on planetary orbiters to conduct direct, passive energy-dispersive x-ray fluorescence measurements of planetary surfaces through measuring the emitted X-Ray fluorescence induced by solar x-rays and high energy particles. Because the Sun is a highly variable radiation source, the intensity of solar X-Ray radiation has to be monitored constantly to allow for comparison and signal calibration of X-Ray radiation from lunar surface materials. Measurements are obtained by indirectly monitoring incident solar x-rays emitted from a calibration sample. This has the additional advantage of minimizing the risk of detector overload and damage during extreme solar events such as high-energy solar flares and particle storms as only the sample targets receive the higher radiation load directly (while the monitor is never directly pointing towards the Sun). Quantitative data are being obtained and can be subsequently analysed through synchronous measurement of fluorescence of the Moon's surface by the XRF-S main instrument and the emitted x-ray fluorescence of calibration samples by the XRF-S-ISM (Indirect Solar Monitor). We are currently developing requirements for 3 sample tiles for onboard correction and calibration of XRF-S, each with an area of 3-9 cm2 and a maximum weight of 45 g. This includes development of design concepts, determination of techniques for sample manufacturing, manufacturing and testing of prototypes and statistical analysis of measurement characteristics and quantification of error sources for the advanced prototypes and final samples. Apart from using natural rock samples as calibration sample, we are currently investigating techniques for sample manufacturing including laser sintering of rock-glass on metals, SiO2-stabilized mineral-powders, or artificial volcanic glass. High precision

Proton-induced x-ray fluorescence CT imaging

PubMed Central

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

2015-01-01

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bunn, Amoret L.; Fritz, Brad G.; Wellman, Dawn M.

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 inmore » the planning for the characterization activities in the RI/FS.« less

Online X-ray Fluorescence (XRF) Analysis of Heavy Metals in Pulverized Coal on a Conveyor Belt.

PubMed

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.

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

PubMed Central

Todd, A C; Chettle, D R

1994-01-01

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

X-Ray Fluorescence Imaging of Ancient Artifacts

NASA Astrophysics Data System (ADS)

Thorne, Robert; Geil, Ethan; Hudson, Kathryn; Crowther, Charles

2011-03-01

Many archaeological artifacts feature inscribed and/or painted text or figures which, through erosion and aging, have become difficult or impossible to read with conventional methods. Often, however, the pigments in paints contain metallic elements, and traces may remain even after visible markings are gone. A promising non-destructive technique for revealing these remnants is X-ray fluorescence (XRF) imaging, in which a tightly focused beam of monochromatic synchrotron radiation is raster scanned across a sample. At each pixel, an energy-dispersive detector records a fluorescence spectrum, which is then analyzed to determine element concentrations. In this way, a map of various elements is made across a region of interest. We have succesfully XRF imaged ancient Greek, Roman, and Mayan artifacts, and in many cases, the element maps have revealed significant new information, including previously invisible painted lines and traces of iron from tools used to carve stone tablets. X-ray imaging can be used to determine an object's provenance, including the region where it was produced and whether it is authentic or a copy.

X-Ray Fluorescence (XRF) to identify chemical analysis of minerals in Buton island, SE Sulawesi, Indonesia

NASA Astrophysics Data System (ADS)

Jamaluddin; Darwis, A.; Massinai, M. A.

2018-02-01

Asbuton as natural rock asphalt consists of a granular material; usually limestone or sandstone. In its natural state, it contains bitumen intimately dispersed throughout its mass, while the remainder of the material is a solid mineral matter. This research was conducted in Sorowalio, Buton Regency, Southeast Sulawesi province, Indonesia. This study aims to determine the content and the percentage of minerals contained in the rocks by using X-Ray Fluorescence (XRF). The method of research is a preliminary survey, sampling and laboratory analysis. XRF reports chemical composition, including Si (quartz) and Ca (calcite). The results indicate the content and the percentage of element dominate the rock sample is Fe2O3, MgO, CaO, and SiO2. Research results using XRF show that there are four metal oxide dominant elements. Hematite (Fe2O3) is dominant in all locations of sampling. Magnesium oxide (MgO) has the highest levels found in sample number six and the lowest is in sample number five. Silicates (SiO) has the highest levels at sample number six and the lowest in sample number seven. Calcium oxide (CaO) is dominant in all sampling locations. The sample of asbuton contains 37.90% asphalt, 43.28% carbonate, and18.82% other minerals.

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

NASA Technical Reports Server (NTRS)

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.

Data precision of X-ray fluorescence (XRF) scanning of discrete samples with the ITRAX XRF core-scanner exemplified on loess-paleosol samples

NASA Astrophysics Data System (ADS)

Profe, Jörn; Ohlendorf, Christian

2017-04-01

XRF-scanning is the state-of-the-art technique for geochemical analyses in marine and lacustrine sedimentology for more than a decade. However, little attention has been paid to data precision and technical limitations so far. Using homogenized, dried and powdered samples (certified geochemical reference standards and samples from a lithologically-contrasting loess-paleosol sequence) minimizes many adverse effects that influence the XRF-signal when analyzing wet sediment cores. This allows the investigation of data precision under ideal conditions and documents a new application of the XRF core-scanner technology at the same time. Reliable interpretations of XRF results require data precision evaluation of single elements as a function of X-ray tube, measurement time, sample compaction and quality of peak fitting. Ten-fold measurement of each sample constitutes data precision. Data precision of XRF measurements theoretically obeys Poisson statistics. Fe and Ca exhibit largest deviations from Poisson statistics. The same elements show the least mean relative standard deviations in the range from 0.5% to 1%. This represents the technical limit of data precision achievable by the installed detector. Measurement times ≥ 30 s reveal mean relative standard deviations below 4% for most elements. The quality of peak fitting is only relevant for elements with overlapping fluorescence lines such as Ba, Ti and Mn or for elements with low concentrations such as Y, for example. Differences in sample compaction are marginal and do not change mean relative standard deviation considerably. Data precision is in the range reported for geochemical reference standards measured by conventional techniques. Therefore, XRF scanning of discrete samples provide a cost- and time-efficient alternative to conventional multi-element analyses. As best trade-off between economical operation and data quality, we recommend a measurement time of 30 s resulting in a total scan time of 30 minutes

Analysis of Historical Coins by X-ray Fluorescence

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

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

PubMed Central

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

2013-01-01

Purpose: To develop a proof-of-principle L-shell x-ray fluorescence (XRF) imaging system that locates and quantifies sparse concentrations of gold nanoparticles (GNPs) using a benchtop polychromatic x-ray source and a silicon (Si)-PIN diode x-ray detector system. Methods: 12-mm-diameter water-filled cylindrical tubes with GNP concentrations of 20, 10, 5, 0.5, 0.05, 0.005, and 0 mg/cm3 served as calibration phantoms. An imaging phantom was created using the same cylindrical tube but filled with tissue-equivalent gel containing structures mimicking a GNP-loaded blood vessel and approximately 1 cm3 tumor. Phantoms were irradiated by a 3-mm-diameter pencil-beam of 62 kVp x-rays filtered by 1 mm aluminum. Fluorescence/scatter photons from phantoms were detected at 90° with respect to the beam direction using a Si-PIN detector placed behind a 2.5-mm-diameter lead collimator. The imaging phantom was translated horizontally and vertically in 0.3-mm steps to image a 6 mm × 15 mm region of interest (ROI). For each phantom, the net L-shell XRF signal from GNPs was extracted from background, and then corrected for detection efficiency and in-phantom attenuation using a fluorescence-to-scatter normalization algorithm. Results: XRF measurements with calibration phantoms provided a calibration curve showing a linear relationship between corrected XRF signal and GNP mass per imaged voxel. Using the calibration curve, the detection limit (at the 95% confidence level) of the current experimental setup was estimated to be a GNP mass of 0.35 μg per imaged voxel (1.73 × 10−2 cm3). A 2D XRF map of the ROI was also successfully generated, reasonably matching the known spatial distribution as well as showing the local variation of GNP concentrations. Conclusions:L-shell XRF imaging can be a highly sensitive tool that has the capability of simultaneously imaging the spatial distribution and determining the local concentration of GNPs presented on the order of parts-per-million level

Portable X-ray diffractometer equipped with XRF for archaeometry

NASA Astrophysics Data System (ADS)

Uda, M.; Ishizaki, A.; Satoh, R.; Okada, K.; Nakajima, Y.; Yamashita, D.; Ohashi, K.; Sakuraba, Y.; Shimono, A.; Kojima, D.

2005-09-01

A portable X-ray diffractometer equipped with an X-ray fluorescence spectrometer was improved so as to get a diffraction pattern and a fluorescence spectrum simultaneously in air from one and the same small area on a specimen. Here, diffraction experiments were performed in two modes, i.e. an angle rotation mode and an energy dispersive mode. In the latter a diffraction pattern and a fluorescence spectrum were simultaneously recorded in a short time, 100 s or less, on one display. The diffractometer was tested in the field to confirm its performance. Targets chosen for this purpose were a bronze mirror from the Eastern Han Dynasty (25-220), and a stupa and its pedestal which are part of the painted statue of "Tamonten holding a stupa" from the Heian Period (794-1192), enshrined in the Engyouji temple founded in 996. The bronze mirror was identified as a product of the Han Dynasty from its chemical composition and the existence of the δ phase in the Cu-Sn alloy. The stupa and its pedestal were decorated with gold powder and gold leaf, respectively. From the XRF data of the pedestal, the underlying layer of gold leaf seems to have been painted with emerald green.

Analysis of heterogeneous gallstones using laser-induced breakdown spectroscopy (LIBS) and wavelength dispersive X-ray fluorescence (WD-XRF).

PubMed

Jaswal, Brij Bir S; Kumar, Vinay; Sharma, Jitendra; Rai, Pradeep K; Gondal, Mohammed A; Gondal, Bilal; Singh, Vivek K

2016-04-01

Laser-induced breakdown spectroscopy (LIBS) is an emerging analytical technique with numerous advantages such as rapidity, multi-elemental analysis, no specific sample preparation requirements, non-destructiveness, and versatility. It has been proven to be a robust elemental analysis tool attracting interest because of being applied to a wide range of materials including biomaterials. In this paper, we have performed spectroscopic studies on gallstones which are heterogeneous in nature using LIBS and wavelength dispersive X-ray fluorescence (WD-XRF) techniques. It has been observed that the presence and relative concentrations of trace elements in different kind of gallstones (cholesterol and pigment gallstones) can easily be determined using LIBS technique. From the experiments carried out on gallstones for trace elemental mapping and detection, it was found that LIBS is a robust tool for such biomedical applications. The stone samples studied in the present paper were classified using the Fourier transform infrared (FTIR) spectroscopy. WD-XRF spectroscopy has been applied for the qualitative and quantitative analysis of major and trace elements present in the gallstone which was compared with the LIBS data. The results obtained in the present paper show interesting prospects for LIBS and WD-XRF to study cholelithiasis better.

Elemental analysis of granite by instrumental neutron activation analysis (INAA) and X-ray fluorescence analysis (XRF).

PubMed

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.

Innovative instrumentation for mineralogical and elemental analyses of solid extraterrestrial surfaces: The Backscatter Moessbauer Spectrometer/X Ray Fluorescence analyzer (BaMS/XRF)

NASA Technical Reports Server (NTRS)

Shelfer, T. D.; Morris, Richard V.; Nguyen, T.; Agresti, D. G.; Wills, E. L.

1994-01-01

We have developed a four-detector research-grade backscatter Moessbauer spectrometer (BaMS) instrument with low resolution x-ray fluorescence analysis (XRF) capability. A flight-qualified instrument based on this design would be suitable for use on missions to the surfaces of solid solar-system objects (Moon, Mars, asteroids, etc.). Target specifications for the flight instrument are as follows: mass less than 500 g; volumes less than 300 cu cm; and power less than 2 W. The BaMS/XRF instrument would provide data on the oxidation state of iron and its distribution among iron-bearing mineralogies and elemental composition information. This data is a primary concern for the characterization of extraterrestrial surface materials.

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

DOE PAGES

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

2015-01-01

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

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

PubMed

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

2015-05-01

Trace metals play critical roles in a variety of systems, ranging from cells to photovoltaics. X-Ray Fluorescence (XRF) microscopy using X-ray excitation provides one of the highest sensitivities available for imaging the distribution of trace metals at sub-100 nm resolution. With the growing availability and increasing performance of synchrotron light source based instruments and X-ray nanofocusing optics, and with improvements in energy-dispersive XRF detectors, what are the factors that limit trace element detectability? To address this question, we describe an analytical model for the total signal incident on XRF detectors with various geometries, including the spectral response of energy dispersive detectors. This model agrees well with experimentally recorded X-ray fluorescence spectra, and involves much shorter calculation times than with Monte Carlo simulations. With such a model, one can estimate the signal when a trace element is illuminated with an X-ray beam, and when just the surrounding non-fluorescent material is illuminated. From this signal difference, a contrast parameter can be calculated and this can in turn be used to calculate the signal-to-noise ratio (S/N) for detecting a certain elemental concentration. We apply this model to the detection of trace amounts of zinc in biological materials, and to the detection of small quantities of arsenic in semiconductors. We conclude that increased detector collection solid angle is (nearly) always advantageous even when considering the scattered signal. However, given the choice between a smaller detector at 90° to the beam versus a larger detector at 180° (in a backscatter-like geometry), the 90° detector is better for trace element detection in thick samples, while the larger detector in 180° geometry is better suited to trace element detection in thin samples. Copyright © 2015. Published by Elsevier B.V.

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

PubMed Central

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

2016-01-01

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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

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

NASA Astrophysics Data System (ADS)

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.

Iodine X-ray fluorescence computed tomography system utilizing a cadmium telluride detector in conjunction with a cerium-target tube

NASA Astrophysics Data System (ADS)

Hagiwara, Osahiko; Watanabe, Manabu; Sato, Eiichi; Matsukiyo, Hiroshi; Osawa, Akihiro; Enomoto, Toshiyuki; Nagao, Jiro; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2011-06-01

An X-ray fluorescence computed tomography system (XRF-CT) is useful for determining the main atoms in objects. To detect iodine atoms without using a synchrotron, we developed an XRF-CT system utilizing a cadmium telluride (CdTe) detector and a cerium X-ray generator. CT is performed by repeated linear scans and rotations of an object. When cerium K-series characteristic X-rays are absorbed by iodine atoms in objects, iodine K fluorescence is produced from atoms and is detected by the CdTe detector. Next, event signals of X-ray photons are produced with the use of charge-sensitive and shaping amplifiers. Iodine Kα fluorescence is isolated using a multichannel analyzer, and the number of photons is counted using a counter card. In energy-dispersive XRF-CT, the tube voltage and tube current were 70 kV and 0.40 mA, respectively, and the X-ray intensity was 115.3 μGy/s at a distance of 1.0 m from the source. The demonstration of XRF-CT was carried out by the selection of photons in an energy range from 27.5 to 29.5 keV with a photon-energy resolution of 1.2 keV.

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

USGS Publications Warehouse

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

1990-01-01

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

Analytical possibilities of different X-ray fluorescence systems for determination of trace elements in aqueous samples pre-concentrated with carbon nanotubes

NASA Astrophysics Data System (ADS)

Marguí, E.; Zawisza, B.; Skorek, R.; Theato, T.; Queralt, I.; Hidalgo, M.; Sitko, R.

2013-10-01

This study was aimed to achieve improved instrumental sensitivity and detection limits for multielement determination of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Pb and Cd in liquid samples by using different X-ray fluorescence (XRF) configurations (a benchtop energy-dispersive X-ray fluorescence spectrometer, a benchtop polarised energy-dispersive X-ray fluorescence spectrometer and a wavelength-dispersive X-ray fluorescence spectrometer). The preconcentration of metals from liquid solutions consisted on a solid-phase extraction using carbon nanotubes (CNTs) as solid sorbents. After the extraction step, the aqueous sample was filtered and CNTs with the absorbed elements were collected onto a filter paper which was directly analyzed by XRF. The calculated detection limits in all cases were in the low ng mL- 1 range. Nevertheless, results obtained indicate the benefits, in terms of sensitivity, of using polarized X-ray sources using different secondary targets in comparison to conventional XRF systems, above all if Cd determination is required. The developed methodologies, using the aforementioned equipments, have been applied for multielement determination in water samples from an industrial area of Poland.

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

ERIC Educational Resources Information Center

Palmer, Peter T.

2011-01-01

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

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

PubMed

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

2013-08-01

To develop a proof-of-principle L-shell x-ray fluorescence (XRF) imaging system that locates and quantifies sparse concentrations of gold nanoparticles (GNPs) using a benchtop polychromatic x-ray source and a silicon (Si)-PIN diode x-ray detector system. 12-mm-diameter water-filled cylindrical tubes with GNP concentrations of 20, 10, 5, 0.5, 0.05, 0.005, and 0 mg∕cm3 served as calibration phantoms. An imaging phantom was created using the same cylindrical tube but filled with tissue-equivalent gel containing structures mimicking a GNP-loaded blood vessel and approximately 1 cm3 tumor. Phantoms were irradiated by a 3-mm-diameter pencil-beam of 62 kVp x-rays filtered by 1 mm aluminum. Fluorescence∕scatter photons from phantoms were detected at 90° with respect to the beam direction using a Si-PIN detector placed behind a 2.5-mm-diameter lead collimator. The imaging phantom was translated horizontally and vertically in 0.3-mm steps to image a 6 mm×15 mm region of interest (ROI). For each phantom, the net L-shell XRF signal from GNPs was extracted from background, and then corrected for detection efficiency and in-phantom attenuation using a fluorescence-to-scatter normalization algorithm. XRF measurements with calibration phantoms provided a calibration curve showing a linear relationship between corrected XRF signal and GNP mass per imaged voxel. Using the calibration curve, the detection limit (at the 95% confidence level) of the current experimental setup was estimated to be a GNP mass of 0.35 μg per imaged voxel (1.73×10(-2) cm3). A 2D XRF map of the ROI was also successfully generated, reasonably matching the known spatial distribution as well as showing the local variation of GNP concentrations. L-shell XRF imaging can be a highly sensitive tool that has the capability of simultaneously imaging the spatial distribution and determining the local concentration of GNPs presented on the order of parts-per-million level within subcentimeter-sized ex vivo

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

PubMed

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

2011-06-01

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

Prostate-cancer diagnosis by non-invasive prostatic Zinc mapping using X-Ray Fluorescence (XRF)

NASA Astrophysics Data System (ADS)

Cortesi, Marco

At present, the major screening tools (PSA, DRE, TRUS) for prostate cancer lack sensitivity and specificity, and none can distinguish between low-grade indolent cancer and high-grade lethal one. The situation calls for the promotion of alternative approaches, with better detection sensitivity and specificity, to provide more efficient selection of patients to biopsy and with possible guidance of the biopsy needles. The prime objective of the present work was the development of a novel non-invasive method and tool for promoting detection, localization, diagnosis and follow-up of PCa. The method is based on in-vivo imaging of Zn distribution in the peripheral zone of the prostate, by a trans-rectal X-ray fluorescence (XRF) probe. Local Zn levels, measured in 1--4 mm3 fresh tissue biopsy segments from an extensive clinical study involving several hundred patients, showed an unambiguous correlation with the histological classification of the tissue (Non-Cancer or PCa), and a systematic positive correlation of its depletion level with the cancer-aggressiveness grade (Gleason classification). A detailed analysis of computer-simulated Zn-concentration images (with input parameters from clinical data) disclosed the potential of the method to provide sensitive and specific detection and localization of the lesion, its grade and extension. Furthermore, it also yielded invaluable data on some requirements, such as the image resolution and counting-statistics, requested from a trans-rectal XRF probe for in-vivo recording of prostatic-Zn maps in patients. By means of systematic table-top experiments on prostate-phantoms comprising tumor-like inclusions, followed by dedicated Monte Carlo simulations, the XRF-probe and its components have been designed and optimized. Multi-parameter analysis of the experimental data confirmed the simulation estimations of the XRF detection system in terms of: delivered dose, counting statistics, scanning resolution, target-volume size and the

Pigment analysis by Raman microscopy and portable X-ray fluorescence (pXRF) of thirteenth to fourteenth century illuminations and cuttings from Bologna

PubMed Central

Clark, Robin J. H.; Jones, Richard; Gibbs, Robert

2016-01-01

Non-destructive pigment analysis by Raman microscopy (RM) and portable X-ray fluorescence (pXRF) has been carried out on some Bolognese illuminations and cuttings chosen to represent the beginnings, evolution and height of Bolognese illuminated manuscript production. Dating to the thirteenth and fourteenth centuries and held in a private collection, the study provides evidence for the pigments generally used in this period. The results, which are compared with those obtained for other north Italian artwork, show the developments in usage of artistic materials and technique. Also addressed in this study is an examination of the respective roles of RM and pXRF analysis in this area of technical art history. This article is part of the themed issue ‘Raman spectroscopy in art and archaeology’. PMID:27799427

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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.

Electroadsorption-assisted direct determination of trace arsenic without interference using transmission X-ray fluorescence spectroscopy.

PubMed

Jiang, Tian-Jia; Guo, Zheng; Liu, Jin-Huai; Huang, Xing-Jiu

2015-08-18

An analytical technique based on electroadsorption and transmission X-ray fluorescence (XRF) for the quantitative determination of arsenic in aqueous solution with ppb-level limits of detection (LOD) is proposed. The approach uses electroadsorption to enhance the sensitivity and LOD of the arsenic XRF response. Amine-functionalized carbonaceous microspheres (NH2-CMSs) are found to be the ideal materials for both the quantitative adsorption of arsenic and XRF analysis due to the basic amine sites on the surface and their noninterference in the XRF spectrum. In electroadsorptive X-ray fluorescence (EA-XRF), arsenic is preconcentrated by a conventional three-electrode system with a positive electricity field around the adsorbents. Then, the quantification of arsenic on the adsorbents is achieved using XRF. The electroadsorption preconcentration can realize the fast transfer of arsenic from the solution to the adsorbents and improve the LOD of conventional XRF compared with directly determining arsenic solution by XRF alone. The sensitivity of 0.09 cnt ppb(-1) is obtained without the interferences from coexisted metal ions in the determination of arsenic, and the LOD is found to be 7 ppb, which is lower than the arsenic guideline value of 10 ppb given by the World Health Organization (WHO). These results demonstrated that XRF coupled with electroadsorption was able to determine trace arsenic in real water sample.

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

PubMed

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.

Capillary Optics Based X-Ray Micro-Imaging Elemental Analysis

NASA Astrophysics Data System (ADS)

Hampai, D.; Dabagov, S. B.; Cappuccio, G.; Longoni, A.; Frizzi, T.; Cibin, G.

2010-04-01

A rapidly developed during the last few years micro-X-ray fluorescence spectrometry (μXRF) is a promising multi-elemental technique for non-destructive analysis. Typically it is rather hard to perform laboratory μXRF analysis because of the difficulty of producing an original small-size X-ray beam as well as its focusing. Recently developed for X-ray beam focusing polycapillary optics offers laboratory X-ray micro probes. The combination of polycapillary lens and fine-focused micro X-ray tube can provide high intensity radiation flux on a sample that is necessary in order to perform the elemental analysis. In comparison to a pinhole, an optimized "X-ray source-op tics" system can result in radiation density gain of more than 3 orders by the value. The most advanced way to get that result is to use the confocal configuration based on two X-ray lenses, one for the fluorescence excitation and the other for the detection of secondary emission from a sample studied. In case of X-ray capillary microfocusing a μXRF instrument designed in the confocal scheme allows us to obtain a 3D elemental mapping. In this work we will show preliminary results obtained with our prototype, a portable X-ray microscope for X-ray both imaging and fluorescence analysis; it enables μXRF elemental mapping simultaneously with X-ray imaging. A prototype of compact XRF spectrometer with a spatial resolution less than 100 μm has been designed.

XRF Experiment for Elementary Surface Analysis

NASA Astrophysics Data System (ADS)

Köhler, E.; Dreißigacker, A.; Fabel, O.; van Gasselt, S.; Meyer, M.

2014-04-01

The proposed X-Ray Fluorescence Instrument Package (XRF-X and XRF-E) is being designed to quantitatively measure the composition and map the distribution of rock-surface materials in order to support the target area selection process for exploration, sampling, and mining. While energydispersive X-Ray fluorescence (EDX) makes use of Solar X-Rays for excitation to probe materials over arbitrary distances (by XRF-X), electron-beam excitation can be used for proximity measurements (by XRF-E) over short-distance of up to about 10 - 20m. This design is targeted at observing and analyzing surface compositions from orbital platforms and it is in particular applicable to all atmosphereless solidsurface bodies. While the instrument design for observing objects in the outer solar system is challenging due to low count rates, the Moon and objects of the asteroid belt usually receive solar X-ray radiation that allows to integrate a statistically reliable data basis. Asteroids are attractive targets and have been visited using X-ray fluorescence instruments by orbiting spacecraft in the past (Itokawa, Eros). They are wellaccessible objects for determining elemental compositions and assessing potential mineral resources.

An optical supernova associated with the X-ray flash XRF 060218.

PubMed

Pian, E; Mazzali, P A; Masetti, N; Ferrero, P; Klose, S; Palazzi, E; Ramirez-Ruiz, E; Woosley, S E; Kouveliotou, C; Deng, J; Filippenko, A V; Foley, R J; Fynbo, J P U; Kann, D A; Li, W; Hjorth, J; Nomoto, K; Patat, F; Sauer, D N; Sollerman, J; Vreeswijk, P M; Guenther, E W; Levan, A; O'Brien, P; Tanvir, N R; Wijers, R A M J; Dumas, C; Hainaut, O; Wong, D S; Baade, D; Wang, L; Amati, L; Cappellaro, E; Castro-Tirado, A J; Ellison, S; Frontera, F; Fruchter, A S; Greiner, J; Kawabata, K; Ledoux, C; Maeda, K; Møller, P; Nicastro, L; Rol, E; Starling, R

2006-08-31

Long-duration gamma-ray bursts (GRBs) are associated with type Ic supernovae that are more luminous than average and that eject material at very high velocities. Less-luminous supernovae were not hitherto known to be associated with GRBs, and therefore GRB-supernovae were thought to be rare events. Whether X-ray flashes--analogues of GRBs, but with lower luminosities and fewer gamma-rays--can also be associated with supernovae, and whether they are intrinsically 'weak' events or typical GRBs viewed off the axis of the burst, is unclear. Here we report the optical discovery and follow-up observations of the type Ic supernova SN 2006aj associated with X-ray flash XRF 060218. Supernova 2006aj is intrinsically less luminous than the GRB-supernovae, but more luminous than many supernovae not accompanied by a GRB. The ejecta velocities derived from our spectra are intermediate between these two groups, which is consistent with the weakness of both the GRB output and the supernova radio flux. Our data, combined with radio and X-ray observations, suggest that XRF 060218 is an intrinsically weak and soft event, rather than a classical GRB observed off-axis. This extends the GRB-supernova connection to X-ray flashes and fainter supernovae, implying a common origin. Events such as XRF 060218 are probably more numerous than GRB-supernovae.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

2016-09-22

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

X-ray fluorescence beamline at the LNLS: Current instrumentation and future developments (abstract)

NASA Astrophysics Data System (ADS)

Pérez, C. A.; Bueno, M. I. S.; Neuenshwander, R. T.; Sánchez, H. J.; Tolentino, H.

2002-03-01

The x-ray fluorescence (XRF) beamline, constructed at the Brazilian National Synchrotron Radiation Laboratory (LNLS-http://www.lnls.br), has been operating for the external users since August of 1998 (C. A. Pérez et al., Proc. of the European Conference on Energy Dispersive X-Ray Spectrometry, Bologna, Italy, 1998, pp. 125-129). The synchrotron source for this beamline is the D09B (15°) dipole magnet of the LNLS storage ring. Two main experimental setups are mounted at the XRF beamline. One consists of a high vacuum chamber adapted to carry out experiments in grazing excitation conditions. This allows chemical trace and ultratrace element determination on several samples, mainly coming from environmental and biological sciences. Another setup consists of an experimental station, operated in air, in which x-ray fluorescence analysis with spatial resolution can be done. This station is equipped with a fine conical capillary, capable of achieving 20 μm spatial resolution, and with an optical microscope in order to select the region of interest on the sample surface. In this work, the main characteristic of the beamline, experimental stations as well as the description of some new experimental facilities will be given. Future development in the instrumentation focuses on an appropriate x-ray optic to be able to carry out chemical trace analysis of light elements using the total x-ray fluorescence technique. Also, chemical mapping below 10 μm spatial resolution, while keeping high flux of photon on the sample, will be achieved by using the Kirkpatrick-Baez x-ray microfocusing optic.

Preparation and characterization of polymer layer systems for validation of 3D Micro X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Schaumann, Ina; Malzer, Wolfgang; Mantouvalou, Ioanna; Lühl, Lars; Kanngießer, Birgit; Dargel, Rainer; Giese, Ulrich; Vogt, Carla

2009-04-01

For the validation of the quantification of the newly-developed method of 3D Micro X-ray fluorescence spectroscopy (3D Micro-XRF) samples with a low average Z matrix and minor high Z elements are best suited. In a light matrix the interferences by matrix effects are minimized so that organic polymers are appropriate as basis for analytes which are more easily detected by X-ray fluorescence spectroscopy. Polymer layer systems were assembled from single layers of ethylene-propylene-diene rubber (EPDM) filled with changing concentrations of silica and zinc oxide as inorganic additives. Layer thicknesses were in the range of 30-150 μm. Before the analysis with 3D Micro-XRF all layers have been characterized by scanning micro-XRF with regard to filler dispersion, by infrared microscopy and light microscopy in order to determine the layer thicknesses and by ICP-OES to verify the concentration of the X-ray sensitive elements in the layers. With the results obtained for stacked polymer systems the validity of the analytical quantification model for the determination of stratified materials by 3D Micro-XRF could be demonstrated.

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

NASA Astrophysics Data System (ADS)

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

2016-04-01

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

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

NASA Astrophysics Data System (ADS)

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

1995-01-01

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

Cancer diagnosis using a conventional x-ray fluorescence camera with a cadmium-telluride detector

NASA Astrophysics Data System (ADS)

Sato, Eiichi; Enomoto, Toshiyuki; Hagiwara, Osahiko; Abudurexiti, Abulajiang; Sato, Koetsu; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2011-10-01

X-ray fluorescence (XRF) analysis is useful for mapping various atoms in objects. Bremsstrahlung X-rays are selected using a 3.0 mm-thick aluminum filter, and these rays are absorbed by indium, cerium and gadolinium atoms in objects. Then XRF is produced from the objects, and photons are detected by a cadmium-telluride detector. The Kα photons are discriminated using a multichannel analyzer, and the number of photons is counted by a counter card. The objects are moved and scanned by an x-y stage in conjunction with a two-stage controller, and X-ray images obtained by atomic mapping are shown on a personal computer monitor. The scan steps of the x and y axes were both 2.5 mm, and the photon-counting time per mapping point was 0.5 s. We carried out atomic mapping using the X-ray camera, and Kα photons from cerium and gadolinium atoms were produced from cancerous regions in nude mice.

X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

NASA Astrophysics Data System (ADS)

Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

2011-12-01

The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I

X-ray Fluorescence Spectroscopy of Pre-Federal American Currency

NASA Astrophysics Data System (ADS)

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).

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

Analysis of sculptures using XRF and X-ray radiography

NASA Astrophysics Data System (ADS)

Calza, C.; Oliveira, D. F.; Freitas, R. P.; Rocha, H. S.; Nascimento, J. R.; Lopes, R. T.

2015-11-01

This work reports the analysis of two sacred images on polychrome wood using X-ray Radiography and Energy Dispersive X-Ray Fluorescence. The first case is the analysis of a sculpture portraying Saint Sebastian, the patron saint of Rio de Janeiro, which is considered the second most ancient sacred image of Brazil. This sculpture was made in Portugal and was transported to Brazil by Estácio Sá, founder of the city of Rio de Janeiro, in 1565. Nowadays, it is located on the main altar of the Church of Capuchin Friars. The second case is the analysis of a sculpture representing Our Lady of Conception, which is located in the D. João VI Museum (EBA/UFRJ, Rio de Janeiro). The objective of these analyses was to evaluate the general conditions of the sculptures, identifying possible problems and internal damages, areas that revealed signs of previous retouchings and the materials and pigments employed by the artists, in order to assist its restoration procedures. EDXRF measurements were carried out with a portable system, developed at the Nuclear Instrumentation Laboratory, consisting of a Si-PIN XR-100CR detector from Amptek and an Oxford TF3005 X-ray tube with W anode. An X-ray source, a CR System GE CR50P and IP detectors were used to perform the radiographs. The XRF analysis of the sculptures identified the original pigments in both cases and the radiographic images revealed details of the manufacture; restored regions; extensive use of lead white; presence of cracks on the wood; use of nails and spikes, etc.

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

NASA Technical Reports Server (NTRS)

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

1986-01-01

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

Elemental analysis using a handheld X-Ray fluorescence spectrometer

USGS Publications Warehouse

Groover, Krishangi D.; Izbicki, John

2016-06-24

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

Quantification of zinc-porphyrin in dry-cured ham products by spectroscopic methods Comparison of absorption, fluorescence and X-ray fluorescence spectroscopy.

PubMed

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 (<0.1ppm). In addition, XRF spectroscopy provides further information regarding other trace elements and can therefore be advantageous in this aspect. This study also focused on XRF determination of Fe in the extracts and as no detectable Fe was found in the three types of 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.

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

NASA Technical Reports Server (NTRS)

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

1996-01-01

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

Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

PubMed

Chung, Frank H

2017-05-01

For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

Conventional X-ray fluorescence camera with a cadmium-telluride detector and its application to cancer diagnosis

NASA Astrophysics Data System (ADS)

Enomoto, Toshiyuki; Sato, Eiichi; Abderyim, Purkhet; Abudurexiti, Abulajiang; Hagiwara, Osahiko; Matsukiyo, Hiroshi; Osawa, Akihiro; Watanabe, Manabu; Nagao, Jiro; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2011-04-01

X-ray fluorescence (XRF) analysis is useful for mapping various molecules in objects. Bremsstrahlung X-rays are selected using a 3.0-mm-thick aluminum filter, and these rays are absorbed by iodine, cerium, and gadolinium molecules in objects. Next, XRF is produced from the objects, and photons are detected by a cadmium-telluride detector. The Kα photons are discriminated using a multichannel analyzer, and the number of photons is counted by a counter card. The objects are moved and scanned by an x- y stage in conjunction with a two-stage controller, and X-ray images obtained by molecular mapping are shown on a personal computer monitor. The scan steps of x and y axes were both 2.5 mm, and the photon-counting time per mapping point was 0.5 s. We carried out molecular mapping using the X-ray camera, and Kα photons from cerium and gadolinium molecules were produced from cancerous regions in nude mice.

Synchrotron Radiation μ-X Ray Fluorescence on Multicellular Tumor Spheroids

NASA Astrophysics Data System (ADS)

Burattini, E.; Cinque, G.; Bellisola, G.; Fracasso, G.; Monti, F.; Colombatti, M.

2003-01-01

Synchrotron Radiation micro X-Ray Fluorescence (SR μ-XRF) was applied for the first time to map the trace element content on Multicellular Tumor Spheroids (MTS), i.e. human cell clusters used as an in vitro model for testing micrometastases responses to antitumoral drugs. In particular, immunotoxin molecules composed of a carrier protein (Transferrin) bound to a powerful cytotoxin (Ricin A), were here considered as representatives of a class of therapheutic macromolecules used in cancer theraphy. Spheroids included in polyacrylamide gel and placed inside quartz capillaries were studied at the ESRF ID22 beamline using a 15 keV monochromatic photon microbeam. Elemental maps (of Fe, Cu, Zn and Pb) on four groups of spheroids grown under different conditions were studied: untreated, treated only with the carrier molecule or with the toxin alone, and with the complete immunotoxin molecule (carrier+toxin). The results indicate that the distribution of Zn and, to some extent, Cu in the spheroid cells is homogeneous and independent of the treatment type. Total Reflection X-Ray Fluorescence (TR-XRF) was also applied to quantify the average trace element content in the spheroids. Future developments of the technique are finally outlined on the basis of these preliminary results.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sciau, Philippe; Leon, Yoanna; Goudeau, Philippe

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 wouldmore » 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.« less

Characterization of uranium bearing material using x-ray fluorescence and direct gamma-rays measurement techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mujaini, M., E-mail: madihah@uniten.edu.my; Chankow, N.; Yusoff, M. Z.

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) detectormore » 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.« less

Dual x-ray fluorescence spectrometer and method for fluid analysis

DOEpatents

Wilson, Bary W.; Shepard, Chester L.

2005-02-22

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

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

NASA Technical Reports Server (NTRS)

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

2013-01-01

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

MapX: 2D XRF for Planetary Exploration - Image Formation and Optic Characterization

DOE PAGES

Sarrazin, P.; Blake, D.; Gailhanou, M.; ...

2018-04-01

Map-X is a planetary instrument concept for 2D X-Ray Fluorescence (XRF) spectroscopy. The instrument is placed directly on the surface of an object and held in a fixed position during the measurement. The formation of XRF images on the CCD detector relies on a multichannel optic configured for 1:1 imaging and can be analyzed through the point spread function (PSF) of the optic. The PSF can be directly measured using a micron-sized monochromatic X-ray source in place of the sample. Such PSF measurements were carried out at the Stanford Synchrotron and are compared with ray tracing simulations. It is shownmore » that artifacts are introduced by the periodicity of the PSF at the channel scale and the proximity of the CCD pixel size and the optic channel size. A strategy of sub-channel random moves was used to cancel out these artifacts and provide a clean experimental PSF directly usable for XRF image deconvolution.« less

MapX: 2D XRF for Planetary Exploration - Image Formation and Optic Characterization

NASA Astrophysics Data System (ADS)

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

2018-04-01

Map-X is a planetary instrument concept for 2D X-Ray Fluorescence (XRF) spectroscopy. The instrument is placed directly on the surface of an object and held in a fixed position during the measurement. The formation of XRF images on the CCD detector relies on a multichannel optic configured for 1:1 imaging and can be analyzed through the point spread function (PSF) of the optic. The PSF can be directly measured using a micron-sized monochromatic X-ray source in place of the sample. Such PSF measurements were carried out at the Stanford Synchrotron and are compared with ray tracing simulations. It is shown that artifacts are introduced by the periodicity of the PSF at the channel scale and the proximity of the CCD pixel size and the optic channel size. A strategy of sub-channel random moves was used to cancel out these artifacts and provide a clean experimental PSF directly usable for XRF image deconvolution.

MapX: 2D XRF for Planetary Exploration - Image Formation and Optic Characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sarrazin, P.; Blake, D.; Gailhanou, M.

Map-X is a planetary instrument concept for 2D X-Ray Fluorescence (XRF) spectroscopy. The instrument is placed directly on the surface of an object and held in a fixed position during the measurement. The formation of XRF images on the CCD detector relies on a multichannel optic configured for 1:1 imaging and can be analyzed through the point spread function (PSF) of the optic. The PSF can be directly measured using a micron-sized monochromatic X-ray source in place of the sample. Such PSF measurements were carried out at the Stanford Synchrotron and are compared with ray tracing simulations. It is shownmore » that artifacts are introduced by the periodicity of the PSF at the channel scale and the proximity of the CCD pixel size and the optic channel size. A strategy of sub-channel random moves was used to cancel out these artifacts and provide a clean experimental PSF directly usable for XRF image deconvolution.« less

X-ray fluorescence microscopy artefacts in elemental maps of topologically complex samples: Analytical observations, simulation and a map correction method

NASA Astrophysics Data System (ADS)

Billè, Fulvio; Kourousias, George; Luchinat, Enrico; Kiskinova, Maya; Gianoncelli, Alessandra

2016-08-01

XRF spectroscopy is among the most widely used non-destructive techniques for elemental analysis. Despite the known angular dependence of X-ray fluorescence (XRF), topological artefacts remain an unresolved issue when using X-ray micro- or nano-probes. In this work we investigate the origin of the artefacts in XRF imaging of topologically complex samples, which are unresolved problems in studies of organic matter due to the limited travel distances of low energy XRF emission from the light elements. In particular we mapped Human Embryonic Kidney (HEK293T) cells. The exemplary results with biological samples, obtained with a soft X-ray scanning microscope installed at a synchrotron facility were used for testing a mathematical model based on detector response simulations, and for proposing an artefact correction method based on directional derivatives. Despite the peculiar and specific application, the methodology can be easily extended to hard X-rays and to set-ups with multi-array detector systems when the dimensions of surface reliefs are in the order of the probing beam size.

Feasibility of a portable X-ray fluorescence device for bone lead measurements of condor bones.

PubMed

Specht, Aaron J; Parish, Chris N; Wallens, Emma K; Watson, Rick T; Nie, Linda H; Weisskopf, Marc G

2018-02-15

Lead based ammunition is a primary source of lead exposure, especially for scavenging wildlife. Lead poisoning remains the leading cause of diagnosed death for the critically endangered California condors, which are annually monitored via blood tests for lead exposure. The results of these tests are helpful in determining recent exposure in condors and in defining the potential for exposure to other species including humans. Since condors are victim to acute and chronic lead exposure, being able to measure both would lend valuable information on the rates of exposure and accumulation through time. A commercial portable X-ray fluorescence (XRF) device has been optimized to measure bone lead in vivo in humans, but this device could also be valuable for field measurements of bone lead in avian species. In this study, we performed measurements of bone Pb in excised, bare condor bones using inductively coupled plasma mass spectrometry (ICP-MS), a cadmium 109 (Cd-109) K-shell X-ray fluorescence (KXRF) system, and a portable XRF system. Both KXRF and portable XRF bone Pb measurement techniques demonstrated good correlations with ICP-MS results (r=0.93 and r=0.92 respectively), even with increasing skin thickness (r=0.86 between ICP-MS and portable XRF at 1.54mm of soft tissue). In conclusion, our results suggest that a portable XRF could be a useful option for measurement of bone Pb in avian species in the field. Copyright © 2017 Elsevier B.V. All rights reserved.

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

ERIC Educational Resources Information Center

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

2011-01-01

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

Laboratory Scale X-ray Fluorescence Tomography: Instrument Characterization and Application in Earth and Environmental Science.

PubMed

Laforce, Brecht; Vermeulen, Bram; Garrevoet, Jan; Vekemans, Bart; Van Hoorebeke, Luc; Janssen, Colin; Vincze, Laszlo

2016-03-15

A new laboratory scale X-ray fluorescence (XRF) imaging instrument, based on an X-ray microfocus tube equipped with a monocapillary optic, has been developed to perform XRF computed tomography experiments with both higher spatial resolution (20 μm) and a better energy resolution (130 eV @Mn-K(α)) than has been achieved up-to-now. This instrument opens a new range of possible applications for XRF-CT. Next to the analytical characterization of the setup by using well-defined model/reference samples, demonstrating its capabilities for tomographic imaging, the XRF-CT microprobe has been used to image the interior of an ecotoxicological model organism, Americamysis bahia. This had been exposed to elevated metal (Cu and Ni) concentrations. The technique allowed the visualization of the accumulation sites of copper, clearly indicating the affected organs, i.e. either the gastric system or the hepatopancreas. As another illustrative application, the scanner has been employed to investigate goethite spherules from the Cretaceous-Paleogene boundary, revealing the internal elemental distribution of these valuable distal ejecta layer particles.

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

PubMed

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

2016-07-01

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

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

PubMed

Musílek, Ladislav; Cechák, Tomáš; Trojek, Tomáš

2012-07-01

Some characteristic features of X-ray fluorescence (XRF) analysis make it an ideal method for investigations of cultural relics and archaeological finds. It has therefore become a standard method used in archaeometry. Paintings, frescos, manuscripts, pottery, metalwork, glass, and many other objects are analysed with the aim of recognising their materials, production technologies and origin, and for identifying counterfeits. This paper reviews various techniques used in XRF analyses of works of art, summarises the advantages and limitations of the method, and presents some typical examples of its use. The general review is supplemented by some techniques used and some results achieved at CTU-FNSPE in Prague. Copyright © 2011 Elsevier Ltd. All rights reserved.

Electrochemical X-ray fluorescence spectroscopy for trace heavy metal analysis: enhancing X-ray fluorescence detection capabilities by four orders of magnitude.

PubMed

Hutton, Laura A; O'Neil, Glen D; Read, Tania L; Ayres, Zoë J; Newton, Mark E; Macpherson, Julie V

2014-05-06

The development of a novel analytical technique, electrochemical X-ray fluorescence (EC-XRF), is described and applied to the quantitative detection of heavy metals in solution, achieving sub-ppb limits of detection (LOD). In EC-XRF, electrochemical preconcentration of a species of interest onto the target electrode is achieved here by cathodic electrodeposition. Unambiguous elemental identification and quantification of metal concentration is then made using XRF. This simple electrochemical preconcentration step improves the LOD of energy dispersive XRF by over 4 orders of magnitude (for similar sample preparation time scales). Large area free-standing boron doped diamond grown using microwave plasma chemical vapor deposition techniques is found to be ideal as the electrode material for both electrodeposition and XRF due to its wide solvent window, transparency to the XRF beam, and ability to be produced in mechanically robust freestanding thin film form. During electrodeposition it is possible to vary both the deposition potential (Edep) and deposition time (tdep). For the metals Cu(2+) and Pb(2+) the highest detection sensitivities were found for Edep = -1.75 V and tdep (=) 4000 s with LODs of 0.05 and 0.04 ppb achieved, respectively. In mixed Cu(2+)/Pb(2+) solutions, EC-XRF shows that Cu(2+) deposition is unimpeded by Pb(2+), across a broad concentration range, but this is only true for Pb(2+) when both metals are present at low concentrations (10 nM), boding well for trace level measurements. In a dual mixed metal solution, EC-XRF can also be employed to either selectively deposit the metal which has the most positive formal reduction potential, E(0), or exhaustively deplete it from solution, enabling uninhibited detection of the metal with the more negative E(0).

Application of micro-X-ray fluorescence to chemical mapping of polar ice

NASA Astrophysics Data System (ADS)

Fourcade, M. C. Morel; Barnola, J. M.; Susini, J.; Baker, R.; Durand, G.; de Angelis, M.; Duval, P.

Synchrotron-based micro-X-ray fluorescence (μXRF) equipment has been used to analyze impurities in polar ice. A customized sample holder has been developed and the μXRF equipment has been adapted with a thermal control system to keep samples unaltered during analyses. Artificial ice samples prepared from ultra-pure water were analyzed to investigate possible contamination and/or experimental artefacts. Analyses of polar ice from Antarctica (Dome C and Vostok) confirm this μXRF technique is non-destructive and sensitive. Experiments can be reproduced to confirm or refine results by focusing on interesting spots such as crystal grain boundaries or specific inclusions. Integration times and resolution can be adjusted to optimize sensitivity. Investigation of unstable particles is possible due to the short analysis time. In addition to identification of elements in impurities, μXRF is able to determine their speciations. The accuracy and reliability of the results confirm the potential of this technique for research in glaciology.

Laboratory-based characterization of plutonium in soil particles using micro-XRF and 3D confocal XRF

DOE PAGES

McIntosh, Kathryn Gallagher; Cordes, Nikolaus Lynn; Patterson, Brian M.; ...

2015-03-29

The investigation of plutonium (Pu) in a soil matrix is of interest in safeguards, nuclear forensics, and environmental remediation activities. The elemental composition of two plutonium contaminated soil particles was characterized nondestructively using a pair of micro X-ray fluorescence spectrometry (micro-XRF) techniques including high resolution X-ray (hiRX) and 3D confocal XRF. The three dimensional elemental imaging capability of confocal XRF permitted the identification two distinct Pu particles within the samples: one external to the Ferich soil matrix and another co-located with Cu within the soil matrix. The size and morphology of the particles was assessed with X-ray transmission microscopy andmore » micro X-ray computed tomography (micro-CT) providing complementary morphological information. Limits of detection for a 30 μm Pu particle are <10 ng for each of the XRF techniques. Ultimately, this study highlights the capability for lab-based, nondestructive, spatially resolved characterization of heterogeneous matrices on the micrometer scale with nanogram sensitivity.« less

Theoretical modeling of a portable x-ray tube based KXRF system to measure lead in bone.

PubMed

Specht, Aaron J; Weisskopf, Marc G; Nie, Linda Huiling

2017-03-01

K-shell x-ray fluorescence (KXRF) techniques have been used to identify health effects resulting from exposure to metals for decades, but the equipment is bulky and requires significant maintenance and licensing procedures. A portable x-ray fluorescence (XRF) device was developed to overcome these disadvantages, but introduced a measurement dependency on soft tissue thickness. With recent advances to detector technology, an XRF device utilizing the advantages of both systems should be feasible. In this study, we used Monte Carlo simulations to test the feasibility of an XRF device with a high-energy x-ray tube and detector operable at room temperature. We first validated the use of Monte Carlo N-particle transport code (MCNP) for x-ray tube simulations, and found good agreement between experimental and simulated results. Then, we optimized x-ray tube settings and found the detection limit of the high-energy x-ray tube based XRF device for bone lead measurements to be 6.91 µg g -1 bone mineral using a cadmium zinc telluride detector. In conclusion, this study validated the use of MCNP in simulations of x-ray tube physics and XRF applications, and demonstrated the feasibility of a high-energy x-ray tube based XRF for metal exposure assessment.

Theoretical modeling of a portable x-ray tube based KXRF system to measure lead in bone

PubMed Central

Specht, Aaron J; Weisskopf, Marc G; Nie, Linda Huiling

2017-01-01

Objective K-shell x-ray fluorescence (KXRF) techniques have been used to identify health effects resulting from exposure to metals for decades, but the equipment is bulky and requires significant maintenance and licensing procedures. A portable x-ray fluorescence (XRF) device was developed to overcome these disadvantages, but introduced a measurement dependency on soft tissue thickness. With recent advances to detector technology, an XRF device utilizing the advantages of both systems should be feasible. Approach In this study, we used Monte Carlo simulations to test the feasibility of an XRF device with a high-energy x-ray tube and detector operable at room temperature. Main Results We first validated the use of Monte Carlo N-particle transport code (MCNP) for x-ray tube simulations, and found good agreement between experimental and simulated results. Then, we optimized x-ray tube settings and found the detection limit of the high-energy x-ray tube based XRF device for bone lead measurements to be 6.91 μg g−1 bone mineral using a cadmium zinc telluride detector. Significance In conclusion, this study validated the use of MCNP in simulations of x-ray tube physics and XRF applications, and demonstrated the feasibility of a high-energy x-ray tube based XRF for metal exposure assessment. PMID:28169835

First demonstration of iodine mapping in nonliving phantoms using an X-ray fluorescence computed tomography system with a cadmium telluride detector and a tungsten-target tube

NASA Astrophysics Data System (ADS)

Sato, Eiichi; Sato, Yuichi; Ehara, Shigeru; Abudurexiti, Abulajiang; Hagiwara, Osahiko; Matsukiyo, Hiroshi; Osawa, Akihiro; Enomoto, Toshiyuki; Watanabe, Manabu; Nagao, Jiro; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2011-05-01

X-ray fluorescence (XRF) analysis is useful for mapping various atoms in objects, and XRF is emitted by absorbing X-ray photons with energies beyond the K-edge energy of the target atom. Narrow-energy-width bremsstrahlung X-rays are selected using a 3.0-mm-thick aluminum filter. These rays are absorbed by iodine media in objects, and iodine XRF is produced from the iodine atoms. Next, iodine Kα photons are discriminated by a multichannel analyzer and the number of photons is counted by a counter card. CT is performed by repeated linear scans and rotations of an object. The X-ray generator has a 100 μm focus tube with a 0.5-mm-thick beryllium window, and the tube voltage and the current for XRF were 80 kV and 0.50 mA, respectively. The demonstration of XRF-CT for mapping iodine atoms was carried out by selection of photons in an energy range from 27.5 to 29.5 keV with a photon-energy resolution of 1.2 keV.

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

NASA Astrophysics Data System (ADS)

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 <= Z <= 14) using glass polycapillary optics are usually designed and applied to confocal geometry. Two such X-ray optics systems are used in this setup. The first one focuses the primary beam on the sample; the second restricts the field of view of the detector. In order to be able to analyze a wider range of elements especialy with (6 <= Z <= 14), both sample and detector are under vacuum. Depth resolution varies between 100 μm at 1 keV fluorescence energy (Na-Kα) and 30 μm for 17.5 keV (Mo-Kα) [1,2]. In order to improve resolution at energies below 9 keV, our group designed similar spectrometer (in cooperation with PREVAC) but instead of primary polycapillary optics we applied single bounce metallic capillaries optics , designed and manufactured in our Laboratory. The vacuum chumber is currently under construction and is expected to be fully operational in September this year. Single bounce gold capillaries with elliptic internal shape have recently been redesigned and developed in our Laboratory. Surface roughness was reduced up to 0.5 nm and slope error to 0.3 mrad. For these capillaries an expected depth resolution varies from 3 μm (1 keV) and 10 µm for 9 keV (Cu-Kα). The spectrometer equipped with gold capillaries offers the possibility of elemental analysis with better depth resolution than is offerred by glass polycapillaries at energies below 9 keV. Furthermore, we will compare the capabilities and limitations of this spectrometer with others, that use laboratory and/or synchrotron sources. Acknowledgments: This work was supported and co-funded by the European Union as part of the Operational Programme Development of Eastern Poland for

Non-destructive analysis of ancient bimetal swords from western Asia by γ-ray radiography and X-ray fluorescence

NASA Astrophysics Data System (ADS)

Shizuma, Kiyoshi; Kajimoto, Tsuyoshi; Endo, Satoru; Matsugi, Kazuhiro; Arimatsu, Yui; Nojima, Hisashi

2017-09-01

Eight ancient bimetal swords held by Hiroshima University, Japan were analyzed non-destructively through γ-ray radiography and X-ray fluorescence (XRF). 137Cs and 60Co γ-ray irradiation sources were used to obtain transmission images of swords. A scanning radiography method using a 60Co γ-ray source was developed. XRF was used for qualitative elemental analysis of the swords. The presence of iron cores in the hilts of some swords had been observed and it was assumed that the cores were a ritual symbol or had a functional purpose. However, our work reveals that these swords were originally bronze-hilted iron swords and that the rusty blades were replaced with bronze blades to maintain the swords' commercial value as an antique. Consequently, the rest of the iron blade was left in the hilt as an iron tang. The junction of the blade and the guard was soldered and painted to match the patina color. XRF analysis clearly showed that the elemental Sn/Cu ratios of the blades and the hilts were different. These findings are useful for clarifying the later modifications of the swords and are important for interpreting Bronze Age and Iron Age history correctly.

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

PubMed

Li, Xiaoli; Yu, Zhaoshui

2016-05-01

Selenium is both a nutrient and a toxin. Selenium-especially organic selenium-is a core component of human nutrition. Thus, it is very important to measure selenium in biological samples. The limited sensitivity of conventional XRF hampers its widespread use in biological samples. Here, we describe the use of high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-Ray fluorescence spectroscopy (EDXRF) in tandem with a three-dimensional optics design to determine 0.1-5.1μgg(-1) levels of selenium in biological samples. The effects of various experimental parameters such as applied voltage, acquisition time, secondary target and various filters were thoroughly investigated. The detection limit of selenium in biological samples via high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-ray fluorescence spectroscopy was decreased by one order of magnitude versus conventional XRF (Paltridge et al., 2012) and found to be 0.1μg/g. To the best of our knowledge, this is the first report to describe EDXRF measurements of Se in biological samples with important implications for the nutrition and analytical chemistry communities. Copyright © 2016 Elsevier Ltd. All rights reserved.

Spatially resolved synchrotron radiation induced X-ray fluorescence analyses of rare Rembrandt silverpoint drawings

NASA Astrophysics Data System (ADS)

Reiche, I.; Radtke, M.; Berger, A.; Görner, W.; Merchel, S.; Riesemeier, H.; Bevers, H.

2006-05-01

New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (1606 1669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of μg/cm2. Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is together with external micro-proton-induced X-ray emission the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing French German database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection.

The holy grail of soil metal contamination site assessment: reducing risk and increasing confidence of decision making using infield portable X-ray Fluorescence (pXRF) technology

NASA Astrophysics Data System (ADS)

Rouillon, M.; Taylor, M. P.; Dong, C.

2016-12-01

This research assesses the advantages of integrating field portable X-ray Fluorescence (pXRF) technology for reducing the risk and increase confidence of decision making for metal-contaminated site assessments. Metal-contaminated sites are often highly heterogeneous and require a high sampling density to accurately characterize the distribution and concentration of contaminants. The current regulatory assessment approaches rely on a small number of samples processed using standard wet-chemistry methods. In New South Wales (NSW), Australia, the current notification trigger for characterizing metal-contaminated sites require the upper 95% confidence interval of the site mean to equal or exceed the relevant guidelines. The method's low `minimum' sampling requirements can misclassify sites due to the heterogeneous nature of soil contamination, leading to inaccurate decision making. To address this issue, we propose integrating infield pXRF analysis with the established sampling method to overcome sampling limitations. This approach increases the minimum sampling resolution and reduces the 95% CI of the site mean. Infield pXRF analysis at contamination hotspots enhances sample resolution efficiently and without the need to return to the site. In this study, the current and proposed pXRF site assessment methods are compared at five heterogeneous metal-contaminated sites by analysing the spatial distribution of contaminants, 95% confidence intervals of site means, and the sampling and analysis uncertainty associated with each method. Finally, an analysis of costs associated with both the current and proposed methods is presented to demonstrate the advantages of incorporating pXRF into metal-contaminated site assessments. The data shows that pXRF integrated site assessments allows for faster, cost-efficient, characterisation of metal-contaminated sites with greater confidence for decision making.

Development of a combined portable x-ray fluorescence and Raman spectrometer for in situ analysis.

PubMed

Guerra, M; Longelin, S; Pessanha, S; Manso, M; Carvalho, M L

2014-06-01

In this work, we have built a portable X-ray fluorescence (XRF) spectrometer in a planar configuration coupled to a Raman head and a digital optical microscope, for in situ analysis. Several geometries for the XRF apparatus and digital microscope are possible in order to overcome spatial constraints and provide better measurement conditions. With this combined spectrometer, we are now able to perform XRF and Raman measurements in the same point without the need for sample collection, which can be crucial when dealing with cultural heritage objects, as well as forensic analysis. We show the capabilities of the spectrometer by measuring several standard reference materials, as well as other samples usually encountered in cultural heritage, geological, as well as biomedical studies.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT NITON XLT700 SERIES XRF ANALYZER

EPA Science Inventory

The Niton XLt 700 Series (XLt) XRF Services x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at ...

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

NASA Astrophysics Data System (ADS)

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.

Methodological challenges of optical tweezers-based X-ray fluorescence imaging of biological model organisms at synchrotron facilities.

PubMed

Vergucht, Eva; Brans, Toon; Beunis, Filip; Garrevoet, Jan; Bauters, Stephen; De Rijcke, Maarten; Deruytter, David; Janssen, Colin; Riekel, Christian; Burghammer, Manfred; Vincze, Laszlo

2015-07-01

Recently, a radically new synchrotron radiation-based elemental imaging approach for the analysis of biological model organisms and single cells in their natural in vivo state was introduced. The methodology combines optical tweezers (OT) technology for non-contact laser-based sample manipulation with synchrotron radiation confocal X-ray fluorescence (XRF) microimaging for the first time at ESRF-ID13. The optical manipulation possibilities and limitations of biological model organisms, the OT setup developments for XRF imaging and the confocal XRF-related challenges are reported. In general, the applicability of the OT-based setup is extended with the aim of introducing the OT XRF methodology in all research fields where highly sensitive in vivo multi-elemental analysis is of relevance at the (sub)micrometre spatial resolution level.

LabVIEW interface with Tango control system for a multi-technique X-ray spectrometry IAEA beamline end-station at Elettra Sincrotrone Trieste

NASA Astrophysics Data System (ADS)

Wrobel, P. M.; Bogovac, M.; Sghaier, H.; Leani, J. J.; Migliori, A.; Padilla-Alvarez, R.; Czyzycki, M.; Osan, J.; Kaiser, R. B.; Karydas, A. G.

2016-10-01

A new synchrotron beamline end-station for multipurpose X-ray spectrometry applications has been recently commissioned and it is currently accessible by end-users at the XRF beamline of Elettra Sincrotrone Trieste. The end-station consists of an ultra-high vacuum chamber that includes as main instrument a seven-axis motorized manipulator for sample and detectors positioning, different kinds of X-ray detectors and optical cameras. The beamline end-station allows performing measurements in different X-ray spectrometry techniques such as Microscopic X-Ray Fluorescence analysis (μXRF), Total Reflection X-Ray Fluorescence analysis (TXRF), Grazing Incidence/Exit X-Ray Fluorescence analysis (GI-XRF/GE-XRF), X-Ray Reflectometry (XRR), and X-Ray Absorption Spectroscopy (XAS). A LabVIEW Graphical User Interface (GUI) bound with Tango control system consisted of many custom made software modules is utilized as a user-friendly tool for control of the entire end-station hardware components. The present work describes this advanced Tango and LabVIEW software platform that utilizes in an optimal synergistic manner the merits and functionality of these well-established programming and equipment control tools.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT RIGAKU ZSX MINI 11 XRF ANALYZER

EPA Science Inventory

The Rigaku ZSX Mini II (ZSX Mini II) XRF Services x-ray fluorescence (XRF) analyzer was demon-strated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2...

In situ observation of dynamic electrodeposition processes by soft x-ray fluorescence microspectroscopy and keyhole coherent diffractive imaging

NASA Astrophysics Data System (ADS)

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.

Resolving colocalization of bacteria and metal(loid)s on plant root surfaces by combining fluorescence in situ hybridization (FISH) with multiple-energy micro-focused X-ray fluorescence (ME μXRF).

PubMed

Honeker, Linnea K; Root, Robert A; Chorover, Jon; Maier, Raina M

2016-12-01

Metal(loid)-contamination of the environment due to anthropogenic activities is a global problem. Understanding the fate of contaminants requires elucidation of biotic and abiotic factors that influence metal(loid) speciation from molecular to field scales. Improved methods are needed to assess micro-scale processes, such as those occurring at biogeochemical interfaces between plant tissues, microbial cells, and metal(loid)s. Here we present an advanced method that combines fluorescence in situ hybridization (FISH) with synchrotron-based multiple-energy micro-focused X-ray fluorescence microprobe imaging (ME μXRF) to examine colocalization of bacteria and metal(loid)s on root surfaces of plants used to phytostabilize metalliferous mine tailings. Bacteria were visualized on a small root section using SytoBC nucleic acid stain and FISH probes targeting the domain Bacteria and a specific group (Alphaproteobacteria, Gammaproteobacteria, or Actinobacteria). The same root region was then analyzed for elemental distribution and metal(loid) speciation of As and Fe using ME μXRF. The FISH and ME μXRF images were aligned using ImageJ software to correlate microbiological and geochemical results. Results from quantitative analysis of colocalization show a significantly higher fraction of As colocalized with Fe-oxide plaques on the root surfaces (fraction of overlap 0.49±0.19) than to bacteria (0.072±0.052) (p<0.05). Of the bacteria that colocalized with metal(loid)s, Actinobacteria, known for their metal tolerance, had a higher correlation with both As and Fe than Alphaproteobacteria or Gammaproteobacteria. This method demonstrates how coupling these micro-techniques can expand our understanding of micro-scale interactions between roots, metal(loid)s and microbes, information that should lead to improved mechanistic models of metal(loid) speciation and fate. Copyright © 2016 Elsevier B.V. All rights reserved.

Apollo 15 X-ray fluorescence experiment

NASA Technical Reports Server (NTRS)

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

1971-01-01

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

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)

EPA Science Inventory

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...

Proposal for a prototype of portable μXRF spectrometer

NASA Astrophysics Data System (ADS)

Polese, C.; Dabagov, S. B.; Esposito, A.; Liedl, A.; Hampai, D.; Bartùli, C.; Ferretti, M.

2015-07-01

μXRF is a powerful instrument for non-destructive characterization of materials of cultural interest. At the XLab Frascati Laboratory this technique is already well performed thanks to the polyCO set equipment allowing simultaneous μXRF 2D mapping. However, due to the strict demand for in situ analysis in this particular field, a new portable μXRF spectrometer equipped with a full polycapillary lens conjugated with a transmission anode X-ray tube is proposed. Many cultural objects are characterized by elements (Ag, Sn, etc.) with high energy fluorescence K-lines. Thus, the capability of a full lens to deliver a high energy fraction of X-ray spectrum, in order to excite the fluorescence K-lines of such elements, is tested.

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

NASA Astrophysics Data System (ADS)

Chiari, Giacomo; Sarrazin, Philippe; Heginbotham, Arlen

2016-11-01

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

Characterization of Archaeological Sediments Using Fourier Transform Infrared (FT-IR) and Portable X-ray Fluorescence (pXRF): An Application to Formative Period Pyro-Industrial Sites in Pacific Coastal Southern Chiapas, Mexico.

PubMed

Neff, Hector; Bigney, Scott J; Sakai, Sachiko; Burger, Paul R; Garfin, Timothy; George, Richard G; Culleton, Brendan J; Kennett, Douglas J

2016-01-01

Archaeological sediments from mounds within the mangrove zone of far-southern Pacific coastal Chiapas, Mexico, are characterized in order to test the hypothesis that specialized pyro-technological activities of the region's prehistoric inhabitants (salt and ceramic production) created the accumulations visible today. Fourier transform infrared spectroscopy (FT-IR) is used to characterize sediment mineralogy, while portable X-ray fluorescence (pXRF) is used to determine elemental concentrations. Elemental characterization of natural sediments by both instrumental neutron activation analysis (INAA) and pXRF also contribute to understanding of processes that created the archaeological deposits. Radiocarbon dates combined with typological analysis of ceramics indicate that pyro-industrial activity in the mangrove zone peaked during the Late Formative and Terminal Formative periods, when population and monumental activity on the coastal plain and piedmont were also at their peaks. © The Author(s) 2015.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 ourmore » 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.« less

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

NASA Astrophysics Data System (ADS)

Specht, Aaron James

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

A first evaluation of the analytical capabilities of the new X-ray fluorescence facility at International Atomic Energy Agency-Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis

NASA Astrophysics Data System (ADS)

Marguí, Eva; Hidalgo, Manuela; Migliori, Alessandro; Leani, Juan José; Queralt, Ignasi; Kallithrakas-Kontos, Nikolaos; Streli, Christina; Prost, Josef; Karydas, Andreas Germanos

2018-07-01

The aim of the work is to present a systematic evaluation of the analytical capabilities of the new X-ray fluorescence facility jointly operated between the International Atomic Energy Agency and the Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis. The analytical performance of the XRF beamline end-station (IAEAXspe) was systematically evaluated under TXRF excitation geometry by analyzing different types of aqueous (lake, waste and fresh water) and solid (soil, vegetal, biological) certified reference materials using an excitation energy of 13.0 keV (for the purpose of multielemental analysis). The results obtained for both types of samples in terms of limits of detection and accuracy were also compared with those obtained using laboratory X-ray tube based TXRF systems with different features (including Mo and W X-ray tube systems). Taking advantage of the possibility to work under high vacuum, the IAEAXspe set-up instrumental sensitivity was also determined using an excitation energy of 6.2 keV to explore the possibilities for light elements determination. A clear improvement of the element detection limits is achieved when comparing this facility to conventional X-ray tube based TXRF systems highlighting the benefits of using the monoenergetic synchrotron exciting radiation and the ultra-high vacuum chamber in comparison with conventional laboratory systems. The results of the present work are discussed in view of further exploitation of the facility for different environmental and biological related applications.

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)

EPA Science Inventory

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...

Usefulness of a Dual Macro- and Micro-Energy-Dispersive X-Ray Fluorescence Spectrometer to Develop Quantitative Methodologies for Historic Mortar and Related Materials Characterization.

PubMed

García-Florentino, Cristina; Maguregui, Maite; Romera-Fernández, Miriam; Queralt, Ignasi; Margui, Eva; Madariaga, Juan Manuel

2018-05-01

Wavelength dispersive X-ray fluorescence (WD-XRF) spectrometry has been widely used for elemental quantification of mortars and cements. In this kind of instrument, samples are usually prepared as pellets or fused beads and the whole volume of sample is measured at once. In this work, the usefulness of a dual energy dispersive X-ray fluorescence spectrometer (ED-XRF), working at two lateral resolutions (1 mm and 25 μm) for macro and microanalysis respectively, to develop quantitative methods for the elemental characterization of mortars and concretes is demonstrated. A crucial step before developing any quantitative method with this kind of spectrometers is to verify the homogeneity of the standards at these two lateral resolutions. This new ED-XRF quantitative method also demonstrated the importance of matrix effects in the accuracy of the results being necessary to use Certified Reference Materials as standards. The results obtained with the ED-XRF quantitative method were compared with the ones obtained with two WD-XRF quantitative methods employing two different sample preparation strategies (pellets and fused beads). The selected ED-XRF and both WD-XRF quantitative methods were applied to the analysis of real mortars. The accuracy of the ED-XRF results turn out to be similar to the one achieved by WD-XRF, except for the lightest elements (Na and Mg). The results described in this work proved that μ-ED-XRF spectrometers can be used not only for acquiring high resolution elemental map distributions, but also to perform accurate quantitative studies avoiding the use of more sophisticated WD-XRF systems or the acid extraction/alkaline fusion required as destructive pretreatment in Inductively coupled plasma mass spectrometry based procedures.

Feasibility of spectro-photometry in X-rays (SPHINX) from the moon

NASA Astrophysics Data System (ADS)

Sarkar, Ritabrata; Chakrabarti, Sandip Kumar

2010-08-01

Doing space Astronomy on lunar surface has several advantages. We present here feasibility of an All Sky Monitoring Payload for Spectro-photometry in X-rays (SPHINX) which can be placed on a lander on the moon or in a space craft orbiting around the moon. The Si-PIN photo-diodes and CdTe crystals are used to detect solar flares, bright gamma bursts, soft gamma-ray repeaters from space and also X-ray fluorescence (XRF) from lunar surface. We present the complete Geant4 simulation to study the feasibility of such an instrument in presence of Cosmic Diffused X-Ray Background (CDXRB). We find that the signal to noise ratio is sufficient for moderate to bright GRBs (above 5 keV), for the quiet sun (up to 100 keV), solar flares, soft gamma-ray repeaters, X-ray Fluorescence (XRF) of lunar surface etc. This is a low-cost system which is capable of performing multiple tasks while stationed at the natural satellite of our planet.

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

NASA Astrophysics Data System (ADS)

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

2016-08-01

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

High-Sensitivity High-Speed X-ray Fluorescence Scanning Cadmium Telluride Detector for Deep-Portion Cancer Diagnosis Utilizing Tungsten-Kα-Excited Gadolinium Mapping

NASA Astrophysics Data System (ADS)

Yanbe, Yutaka; Sato, Eiichi; Chiba, Hiraku; Maeda, Tomoko; Matsushita, Ryo; Oda, Yasuyuki; Hagiwara, Osahiko; Matsukiyo, Hiroshi; Osawa, Akihiro; Enomoto, Toshiyuki; Watanabe, Manabu; Kusachi, Shinya; Sato, Shigehiro; Ogawa, Akira

2013-09-01

X-ray fluorescence (XRF) analysis is useful for mapping various atoms in objects. Bremsstrahlung X-rays with energies beyond tantalum (Ta) K-edge energy 67.4 keV are absorbed effectively using a 100-µm-thick Ta filter, and the filtered X-rays including tungsten (W) Kα rays are absorbed by gadolinium (Gd) atoms in objects. The Gd XRF is then produced from Gd atoms in the objects and is counted by a cadmium telluride (CdTe) detector. Gd Kα photons with a maximum count rate of 1 kilo counts per second are dispersed using a multichannel analyzer, and the number of photons is counted by a counter card. The distance between the CdTe detector and the object is minimized to 40 mm to increase the count rate. The object is scanned using an x-y stage with a velocity of 5.0 mm/s, and Gd mapping are shown on a computer monitor. The scan steps of the x- and y-axes were both 2.5 mm, and the photon-counting time per mapping point was 0.5 s. We obtained Gd XRF images at high contrast, and Gd Kα photons were easily detected from cancerous regions in a nude mouse placed behind a 20-mm-thick poly(methyl methacrylate) plate.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT XCALIBUR ELVAX XRF ANALYZER

EPA Science Inventory

The Innov-X XT400 Series (XT400) x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kenned...

A Review of the Handheld X-Ray Fluorescence Spectrometer as a Tool for Field Geologic Investigations on Earth and in Planetary Surface Exploration

NASA Technical Reports Server (NTRS)

Young, Kelsey E.; Evans, Cynthia A.; Hodges, Kip V.; Bleacher, Jacob E.; Graff, Trevor G.

2016-01-01

X-ray fluorescence (XRF) spectroscopy is a well-established and commonly used technique in obtaining diagnostic compositional data on geological samples. Recently, developments in X-ray tube and detector technologies have resulted in miniaturized, field-portable instruments that enable new applications both in and out of standard laboratory settings. These applications, however, have not been extensively applied to geologic field campaigns. This study investigates the feasibility of using developing handheld XRF (hXRF) technology to enhance terrestrial field geology, with potential applications in planetary surface exploration missions. We demonstrate that the hXRF is quite stable, providing reliable and accurate data continuously over a several year period. Additionally, sample preparation is proved to have a marked effect on the strategy for collecting and assimilating hXRF data. While the hXRF is capable of obtaining data that are comparable to laboratory XRF analysis for several geologically-important elements (such as Si, Ca, Ti, and K), the instrument is unable to detect other elements (such as Mg and Na) reliably. While this limits the use of the hXRF, especially when compared to laboratory XRF techniques, the hXRF is still capable of providing the field user with significantly improved contextual awareness of a field site, and more work is needed to fully evaluate the potential of this instrument in more complex geologic environments.

Development of a micro-XRF system for biological samples based on proton-induced quasimonochromatic X-rays

NASA Astrophysics Data System (ADS)

Ploykrachang, K.; Hasegawa, J.; Kondo, K.; Fukuda, H.; Oguri, Y.

2014-07-01

We have developed a micro-XRF system based on a proton-induced quasimonochromatic X-ray (QMXR) microbeam for in vivo measurement of biological samples. A 2.5-MeV proton beam impinged normally on a Cu foil target that was slightly thicker than the proton range. The emitted QMXR behind the Cu target was focused with a polycapillary X-ray half lens. For application to analysis of wet or aquatic samples, we prepared a QMXR beam with an incident angle of 45° with respect to the horizontal plane by using a dipole magnet in order to bend the primary proton beam downward by 45°. The focal spot size of the QMXR microbeam on a horizontal sample surface was evaluated to be 250 × 350 μm by a wire scanning method. A microscope camera with a long working distance was installed perpendicular to the sample surface to identify the analyzed position on the sample. The fluorescent radiation from the sample was collected by a Si-PIN photodiode X-ray detector. Using the setup above, we were able to successfully measure the accumulation and distribution of Co in the leaves of a free-floating aquatic plant on a dilute Co solution surface.

Carbon nanotubes allow capture of krypton, barium and lead for multichannel biological X-ray fluorescence imaging

NASA Astrophysics Data System (ADS)

Serpell, Christopher J.; Rutte, Reida N.; Geraki, Kalotina; Pach, Elzbieta; Martincic, Markus; Kierkowicz, Magdalena; de Munari, Sonia; Wals, Kim; Raj, Ritu; Ballesteros, Belén; Tobias, Gerard; Anthony, Daniel C.; Davis, Benjamin G.

2016-10-01

The desire to study biology in situ has been aided by many imaging techniques. Among these, X-ray fluorescence (XRF) mapping permits observation of elemental distributions in a multichannel manner. However, XRF imaging is underused, in part, because of the difficulty in interpreting maps without an underlying cellular `blueprint' this could be supplied using contrast agents. Carbon nanotubes (CNTs) can be filled with a wide range of inorganic materials, and thus can be used as `contrast agents' if biologically absent elements are encapsulated. Here we show that sealed single-walled CNTs filled with lead, barium and even krypton can be produced, and externally decorated with peptides to provide affinity for sub-cellular targets. The agents are able to highlight specific organelles in multiplexed XRF mapping, and are, in principle, a general and versatile tool for this, and other modes of biological imaging.

X-ray Fluorescence Holography: Principles, Apparatus, and Applications

NASA Astrophysics Data System (ADS)

Hayashi, Kouichi; Korecki, Pawel

2018-06-01

X-ray fluorescence holography (XFH) is an atomic structure determination technique that combines the capabilities of X-ray diffraction and X-ray fluorescence spectroscopy. It provides a unique means of gaining fully three-dimensional information about the local atomic structure and lattice site positions of selected elements inside compound samples. In this work, we discuss experimental and theoretical aspects that are essential for the efficient recording and analysis of X-ray fluorescence holograms and review the most recent advances in XFH. We describe experiments performed with brilliant synchrotron radiation as well as with tabletop setups that employ conventional X-ray tubes.

Characterization of fossil remains using XRF, XPS and XAFS spectroscopies

NASA Astrophysics Data System (ADS)

Zougrou, I. M.; Katsikini, M.; Pinakidou, F.; Brzhezinskaya, M.; Papadopoulou, L.; Vlachos, E.; Tsoukala, E.; Paloura, E. C.

2016-05-01

Synchrotron radiation micro-X-Ray Fluorescence (μ-XRF), X-ray photoelectron (XPS) and X-ray Absorption Fine Structure (XAFS) spectroscopies are applied for the study of paleontological findings. More specifically the costal plate of a gigantic terrestrial turtle Titanochelon bacharidisi and a fossilized coprolite of the cave spotted hyena Crocuta crocuta spelaea are studied. Ca L 2,3-edge NEXAFS and Ca 2p XPS are applied for the identification and quantification of apatite and Ca containing minerals. XRF mapping and XAFS are employed for the study of the spatial distribution and speciation of the minerals related to the deposition environment.

A portable x-ray fluorescence instrument for analyzing dust wipe samples for lead: evaluation with field samples.

PubMed

Sterling, D A; Lewis, R D; Luke, D A; Shadel, B N

2000-06-01

Dust wipe samples collected in the field were tested by nondestructive X-ray fluorescence (XRF) followed by laboratory analysis with flame atomic absorption spectrophotometry (FAAS). Data were analyzed for precision and accuracy of measurement. Replicate samples with the XRF show high precision with an intraclass correlation coefficient (ICC) of 0.97 (P<0.0001) and an overall coefficient of variation of 11.6%. Paired comparison indicates no statistical difference (P=0.272) between XRF and FAAS analysis. Paired samples are highly correlated with an R(2) ranging between 0.89 for samples that contain paint chips and 0.93 for samples that do not contain paint chips. The ICC for absolute agreement between XRF and laboratory results was 0.95 (P<0.0001). The relative error over the concentration range of 25 to 14,200 microgram Pb is -12% (95% CI, -18 to -5). The XRF appears to be an excellent method for rapid on-site evaluation of dust wipes for clearance and risk assessment purposes, although there are indications of some confounding when paint chips are present. Copyright 2000 Academic Press.

A new large solid angle multi-element silicon drift detector system for low energy X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Bufon, J.; Schillani, S.; Altissimo, M.; Bellutti, P.; Bertuccio, G.; Billè, F.; Borghes, R.; Borghi, G.; Cautero, G.; Cirrincione, D.; Fabiani, S.; Ficorella, F.; Gandola, M.; Gianoncelli, A.; Giuressi, D.; Kourousias, G.; Mele, F.; Menk, R. H.; Picciotto, A.; Rachevski, A.; Rashevskaya, I.; Sammartini, M.; Stolfa, A.; Zampa, G.; Zampa, N.; Zorzi, N.; Vacchi, A.

2018-03-01

Low-energy X-ray fluorescence (LEXRF) is an essential tool for bio-related research of organic samples, whose composition is dominated by light elements. Working at energies below 2 keV and being able to detect fluorescence photons of lightweight elements such as carbon (277 eV) is still a challenge, since it requires in-vacuum operations to avoid in-air photon absorption. Moreover, the detectors must have a thin entrance window and collect photons at an angle of incidence near 90 degrees to minimize the absorption by the protective coating. Considering the low fluorescence yield of light elements, it is important to cover a substantial part of the solid angle detecting ideally all emitted X-ray fluorescence (XRF) photons. Furthermore, the energy resolution of the detection system should be close to the Fano limit in order to discriminate elements whose XRF emission lines are often very close within the energy spectra. To ensure all these features, a system consisting of four monolithic multi-element silicon drift detectors was developed. The use of four separate detector units allows optimizing the incidence angle on all the sensor elements. The multi-element approach in turn provides a lower leakage current on each anode, which, in combination with ultra-low noise preamplifiers, is necessary to achieve an energy resolution close to the Fano limit. The potential of the new detection system and its applicability for typical LEXRF applications has been proved on the Elettra TwinMic beamline.

An Application of X-Ray Fluorescence as Process Analytical Technology (PAT) to Monitor Particle Coating Processes.

PubMed

Nakano, Yoshio; Katakuse, Yoshimitsu; Azechi, Yasutaka

2018-06-01

An attempt to apply X-Ray Fluorescence (XRF) analysis to evaluate small particle coating process as a Process Analytical Technologies (PAT) was made. The XRF analysis was used to monitor coating level in small particle coating process with at-line manner. The small particle coating process usually consists of multiple coating processes. This study was conducted by a simple coating particles prepared by first coating of a model compound (DL-methionine) and second coating by talc on spherical microcrystalline cellulose cores. The particles with two layered coating are enough to demonstrate the small particle coating process. From the result by the small particle coating process, it was found that the XRF signal played different roles, resulting that XRF signals by first coating (layering) and second coating (mask coating) could demonstrate the extent with different mechanisms for the coating process. Furthermore, the particle coating of the different particle size has also been investigated to evaluate size effect of these coating processes. From these results, it was concluded that the XRF could be used as a PAT in monitoring particle coating processes and become powerful tool in pharmaceutical manufacturing.

Fluorescent scanning x-ray tomography with synchrotron radiation

NASA Astrophysics Data System (ADS)

Takeda, Tohoru; Maeda, Toshikazu; Yuasa, Tetsuya; Akatsuka, Takao; Ito, Tatsuo; Kishi, Kenichi; Wu, Jin; Kazama, Masahiro; Hyodo, Kazuyuki; Itai, Yuji

1995-02-01

Fluorescent scanning (FS) x-ray tomography was developed to detect nonradioactive tracer materials (iodine and gadolinium) in a living object. FS x-ray tomography consists of a silicon (111) channel cut monochromator, an x-ray shutter, an x-ray slit system and a collimator for detection, a scanning table for the target organ, and an x-ray detector with pure germanium. The minimal detectable dose of iodine in this experiment was 100 ng in a volume of 2 mm3 and a linear relationship was shown between the photon counts of a fluorescent x ray and the concentration of iodine contrast material. A FS x-ray tomographic image was clearly obtained with a phantom.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT RONTEC PICOTAX XRF ANALYZER

EPA Science Inventory

The Rontec PicoTAX x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Rec...

Stoichiometry determination of (Pb,La)(Zr,Ti)O3-type nano-crystalline ferroelectric ceramics by wavelength-dispersive X-ray fluorescence spectrometry.

PubMed

Sitko, Rafał; Zawisza, Beata; Kita, Andrzej; Płońska, Małgorzata

2006-07-01

Analysis of small samples of lanthanum-doped lead zirconate titanate (PLZT) by wavelength-dispersive X-ray fluorescence spectrometry (WDXRF) is presented. The powdered material in ca. 30 mg was suspended in water and collected on the membrane filter. The pure oxide standards (PbO, La2O3, ZrO2 and TiO2) were used for calibration. The matrix effects were corrected using a theoretical influence coefficients algorithm for intermediate-thickness specimens. The results from XRF method were compared with the results from the inductively coupled plasma optical emission spectrometry (ICP-OES). Agreement between XRF and ICP-OES analysis was satisfactory and indicates the usefulness of XRF method for stoichiometry determination of PLZT.

Reducing bone lead content by chelation treatment in chronic lead poisoning: an in vivo X-ray fluorescence and bone biopsy study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Batuman, V.; Wedeen, R.P.; Bogden, J.D.

1989-02-01

A stained-glass artist with longstanding exposure to lead presented with neuropsychiatric symptoms. He was evaluated before and after chelation treatment by the CaNa2 EDTA lead mobilization test, iliac crest bone lead measurement, and in vivo tibial X-ray fluorescence (XRF). The three methods showed a progressive fall in body lead stores during chelation therapy in association with improvement in symptoms and a fall in blood lead and zinc protoporphyrin levels. In vivo tibial XRF is a safe, rapid, and noninvasive technique for detecting excessive body lead burdens. XRF measurement of bone lead content is a practical method for monitoring the efficacymore » of therapy as well as for establishing the diagnosis.« less

CubeX: The CubeSAT X-ray Telescope for Elemental Abundance Mapping of Airless Bodies and X-ray Pulsar Navigation

NASA Astrophysics Data System (ADS)

Nittler, L. R.; Hong, J.; Kenter, A.; Romaine, S.; Allen, B.; Kraft, R.; Masterson, R.; Elvis, M.; Gendreau, K.; Crawford, I.; Binzel, R.; Boynton, W. V.; Grindlay, J.; Ramsey, B.

2017-12-01

The surface elemental composition of a planetary body provides crucial information about its origin, geological evolution, and surface processing, all of which can in turn provide information about solar system evolution as a whole. Remote sensing X-ray fluorescence (XRF) spectroscopy has been used successfully to probe the major-element compositions of airless bodies in the inner solar system, including the Moon, near-Earth asteroids, and Mercury. The CubeSAT X-ray Telescope (CubeX) is a concept for a 6U planetary X-ray telescope (36U with S/C), which utilizes Miniature Wolter-I X-ray optics (MiXO), monolithic CMOS and SDD X-ray sensors for the focal plane, and a Solar X-ray Monitor (heritage from the REXIS XRF instrument on NASA's OSIRIS-REx mission). CubeX will map the surface elemental composition of diverse airless bodies by spectral measurement of XRF excited by solar X-rays. The lightweight ( 1 kg) MiXO optics provide sub-arcminute resolution with low background, while the inherently rad-hard CMOS detectors provide improved spectral resolution ( 150 eV) at 0 °C. CubeX will also demonstrate X-ray pulsar timing based deep space navigation (XNAV). Successful XNAV will enable autonomous deep navigation with little to no support from the Deep Space Network, hence lowering the operation cost for many more planetary missions. Recently selected by NASA Planetary Science Deep Space SmallSat Studies, the first CubeX concept, designed to rideshare to the Moon as a secondary spacecraft on a primary mission, is under study in collaboration with the Mission Design Center at NASA Ames Research Center. From high altitude ( 6,000 km) frozen polar circular orbits, CubeX will study > 8 regions ( 110 km) of geological interest on the Moon over one year to produce a high resolution ( 2-3 km) elemental abundance map of each region. The novel focal plane design of CubeX also allows us to evaluate the performance of absolute navigation by sequential observations of several

µ-XANES AND µ-XRF INVESTIGATIONS OF METAL BINDING MECHANISMS IN BIOSOLIDS

EPA Science Inventory

Micro-X-ray fluorescence (µ-XRF) microprobe analysis and micro-X-ray absorption near edge spectroscopy (µ-XANES) were employed to identify Fe and Mn phases and their association with selected toxic elements in two biosolids (limed composted and Nu-Earth) containing low ...

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

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

NASA Technical Reports Server (NTRS)

Rolin, T. D.; Leszczuk, Y.

2008-01-01

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

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF TECHNOLOGIES FOR MEASURING TRACE ELEMENTS IN SOIL AND SEDIMENT OXFORD ED2000 XRF ANALYZER

EPA Science Inventory

The Oxford ED2000 x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recr...

NHEXAS PHASE I ARIZONA STUDY--METALS-XRF IN DUST ANALYTICAL RESULTS

EPA Science Inventory

The Metals-XRF in Dust data set contains X-ray fluorescence (XRF) analytical results for measurements of up to 27 metals in 384 dust samples over 384 households. Samples were taken by collecting dust from the indoor floor areas in the main room and in the bedroom of the primary ...

First use of portable system coupling X-ray diffraction and X-ray fluorescence for in-situ analysis of prehistoric rock art.

PubMed

Beck, L; Rousselière, H; Castaing, J; Duran, A; Lebon, M; Moignard, B; Plassard, F

2014-11-01

Study of prehistoric art is playing a major role in the knowledge of human evolution. Many scientific methods are involved in this investigation including chemical analysis of pigments present on artefacts or applied to cave walls. In the past decades, the characterization of coloured materials was carried on by taking small samples. This procedure had two main disadvantages: slight but existing damage of the paintings and limitation of the number of samples. Thanks to the advanced development of portable systems, in-situ analysis of pigment in cave can be now undertaken without fear for this fragile Cultural Heritage. For the first time, a portable system combining XRD and XRF was used in an underground and archaeological environment for prehistoric rock art studies. In-situ non-destructive analysis of black prehistoric drawings and determination of their composition and crystalline structure were successfully carried out. Original results on pigments used 13,000 years ago in the cave of Rouffignac (France) were obtained showing the use of two main manganese oxides: pyrolusite and romanechite. The capabilities of the portable XRD-XRF system have been demonstrated for the characterization of pigments as well as for the analysis of rock in a cave environment. This first in-situ experiment combining X-ray diffraction and X-ray fluorescence open up new horizons and can fundamentally change our approach of rock art studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Forensic analysis of laser printed ink by X-ray fluorescence and laser-excited plume fluorescence.

PubMed

Chu, Po-Chun; Cai, Bruno Yue; Tsoi, Yeuk Ki; Yuen, Ronald; Leung, Kelvin S Y; Cheung, Nai-Ho

2013-05-07

We demonstrated a minimally destructive two-tier approach for multielement forensic analysis of laser-printed ink. The printed document was first screened using a portable-X-ray fluorescence (XRF) probe. If the results were not conclusive, a laser microprobe was then deployed. The laser probe was based on a two-pulse scheme: the first laser pulse ablated a thin layer of the printed ink; the second laser pulse at 193 nm induced multianalytes in the desorbed ink to fluoresce. We analyzed four brands of black toners. The toners were printed on paper in the form of patches or letters or overprinted on another ink. The XRF probe could sort the four brands if the printed letters were larger than font 20. It could not tell the printing sequence in the case of overprints. The laser probe was more discriminatory; it could sort the toner brands and reveal the overprint sequence regardless of font size while the sampled area was not visibly different from neighboring areas even under the microscope. In terms of general analytical performance, the laser probe featured tens of micrometer lateral resolution and tens to hundreds of nm depth resolution and atto-mole mass detection limits. It could handle samples of arbitrary size and shape and was air compatible, and no sample pretreatment was necessary. It will prove useful whenever high-resolution and high sensitivity 3D elemental mapping is required.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Elvatech, Ltd. ElvaX (ElvaX) x-ray fluorescence (XRF) analyzer distributed in the United States by Xcalibur XRF Services (Xcalibur), was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the ElvaX analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the ElvaX analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as s

Atmospheric Electron-Induced X-Ray Spectrometer (AEXS) Development

NASA Technical Reports Server (NTRS)

Wilcox, Jaroslava Z.; Urgiles, Eduardo; Toda, Risaku; George, Thomas; Douglas, Susanne; Crisp, Joy

2005-01-01

This paper describes the progress in the development of the so-called Atmospheric Electron X-ray Spectrometer (AEXS) instrument in our laboratory at JPL. The AEXS is a novel miniature instrument concept based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam, for non-destructive evaluation of surfaces of samples in situ, in planetary ambient atmosphere. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum within the AEXS electron source from the outside ambient atmosphere. By using a focused electron beam, the impinging electrons on samples in the external atmosphere excite XRF spectra from the irradiated spots with high-to-medium spatial resolution. The XRF spectra are analyzed using an energy-dispersive detector to determine surface elemental composition. The use of high- intensity electron beam results in rapid spectrum acquisition (several minutes), and consequently low energy consumption (several tens of Joules) per acquired XRF spectrum in comparison to similar portable instruments.

Analytical performance of a versatile laboratory microscopic X-ray fluorescence system for metal uptake studies on argillaceous rocks

NASA Astrophysics Data System (ADS)

Gergely, Felicián; Osán, János; Szabó, B. Katalin; Török, Szabina

2016-02-01

Laboratory-scale microscopic X-ray fluorescence (micro-XRF) plays an increasingly important role in various fields where multielemental investigations of samples are indispensable. In case of geological samples, the reasonable detection limits (LOD) and spatial resolutions are necessary to identify the trace element content in microcrystalline level. The present study focuses on the analytical performance of a versatile laboratory-scale micro-XRF system with various options of X-ray sources and detectors to find the optimal experimental configuration in terms of sensitivities and LOD for selected elements in loaded petrographic thin sections. The method was tested for sorption studies involving thin sections prepared from cores of Boda Claystone Formation, which is a potential site for a high-level radioactive waste repository. Loaded ions in the sorption measurements were Cs(I) and Ni(II) chemically representing fission and corrosion products. Based on the collected elemental maps, the correlation between the elements representative of main rock components and the selected loaded ion was studied. For the elements of interest, Cs(I) and Ni(II) low-power iMOXS source with polycapillary and silicon drift detector was found to be the best configuration to reach the optimal LOD values. Laboratory micro-XRF was excellent to identify the responsible key minerals for the uptake of Cs(I). In case of nickel, careful corrections were needed because of the relatively high Ca content of the rock samples. The results were compared to synchrotron radiation micro-XRF.

Joint reconstruction of x-ray fluorescence and transmission tomography

DOE PAGES

Di, Zichao; Chen, Si; Hong, Young Pyo; ...

2017-05-30

X-ray fluorescence tomography is based on the detection of fluorescence x-ray photons produced following x-ray absorption while a specimen is rotated; it provides information on the 3D distribution of selected elements within a sample. One limitation in the quality of sample recovery is the separation of elemental signals due to the finite energy resolution of the detector. Another limitation is the effect of self-absorption, which can lead to inaccurate results with dense samples. To recover a higher quality elemental map, we combine x-ray fluorescence detection with a second data modality: conventional x-ray transmission tomography using absorption. By using these combinedmore » signals in a nonlinear optimization-based approach, we demonstrate the benefit of our algorithm on real experimental data and obtain an improved quantitative reconstruction of the spatial distribution of dominant elements in the sample. Furthermore, compared with single-modality inversion based on x-ray fluorescence alone, this joint inversion approach reduces ill-posedness and should result in improved elemental quantification and better correction of self-absorption.« less

Joint reconstruction of x-ray fluorescence and transmission tomography

PubMed Central

Di, Zichao Wendy; Chen, Si; Hong, Young Pyo; Jacobsen, Chris; Leyffer, Sven; Wild, Stefan M.

2017-01-01

X-ray fluorescence tomography is based on the detection of fluorescence x-ray photons produced following x-ray absorption while a specimen is rotated; it provides information on the 3D distribution of selected elements within a sample. One limitation in the quality of sample recovery is the separation of elemental signals due to the finite energy resolution of the detector. Another limitation is the effect of self-absorption, which can lead to inaccurate results with dense samples. To recover a higher quality elemental map, we combine x-ray fluorescence detection with a second data modality: conventional x-ray transmission tomography using absorption. By using these combined signals in a nonlinear optimization-based approach, we demonstrate the benefit of our algorithm on real experimental data and obtain an improved quantitative reconstruction of the spatial distribution of dominant elements in the sample. Compared with single-modality inversion based on x-ray fluorescence alone, this joint inversion approach reduces ill-posedness and should result in improved elemental quantification and better correction of self-absorption. PMID:28788848

Synchrotron radiation microbeam X-ray fluorescence analysis of zinc concentration in remineralized enamel in situ.

PubMed

Matsunaga, Tsunenori; Ishizaki, Hidetaka; Tanabe, Shuji; Hayashi, Yoshihiko

2009-05-01

Remineralization is an indispensable phenomenon during the natural healing process of enamel decay. The incorporation of zinc (Zn) into enamel crystal could accelerate this remineralization. The present study was designed to investigate the concentration and distribution of Zn in remineralized enamel after gum chewing. The experiment was performed at the Photon Factory. Synchrotron radiation was monochromatized and X-rays were focused into a small beam spot. The X-ray fluorescence (XRF) from the sample was detected with a silicon (Si) (lithium (Li)) detector. X-ray beam energy was tuned to detect Zn. The examined samples were small enamel fragments remineralized after chewing calcium phosphate-containing gum in situ. The incorporation of Zn atom into hydroxyapatite (OHAP), the main component of enamel, was measured using Zn K-edge extended X-ray absorption fine structure (EXAFS) with fluorescence mode at the SPring-8. A high concentration of Zn was detected in a superficial area 10-microm deep of the sectioned enamel after gum chewing. This concentration increased over that in the intact enamel. The atomic distance between Zn and O in the enamel was calculated using the EXAFS data. The analyzed atomic distances between Zn and O in two sections were 0.237 and 0.240 nm. The present experiments suggest that Zn is effectively incorporated into remineralized enamel through the physiological processes of mineral deposition in the oral cavity through gum-chewing and that Zn substitution probably occurred at the calcium position in enamel hydroxyapatite.

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

NASA Astrophysics Data System (ADS)

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.

X-ray Fluorescence Core Scanning of Oman Drilling Project Holes BT1B and GT3A Cores on D/V CHIKYU

NASA Astrophysics Data System (ADS)

Johnson, K. T. M.; Kelemen, P. B.; Michibayashi, K.; Greenberger, R. N.; Koepke, J.; Beinlich, A.; Morishita, T.; Jesus, A. P. M.; Lefay, R.

2017-12-01

The JEOL JSX-3600CA1 energy dispersive X-ray fluorescence core logger (XRF-CL) on the D/V Chikyu provides quantitative element concentrations of scanned cores. Scans of selected intervals are made on an x-y grid with point spacing of 5 mm. Element concentrations for Si, Al, Ti, Ca, Mg, Mn, Fe, Na, K, Cr, Ni, S and Zn are collected for each point on the grid. Accuracy of element concentrations provided by the instrument software is improved by applying empirical correction algorithms. Element concentrations were collected for 9,289 points from twenty-seven core intervals in Hole BT1B (basal thrust) and for 6,389 points from forty core intervals in Hole GT3A (sheeted dike-gabbro transition) of the Oman Drilling Project on the D/V Chikyu XRF-CL during Leg 2 of the Oman Drilling Project in August-September, 2017. The geochemical data are used for evaluating downhole compositional details associated with lithological changes, unit contacts and mineralogical variations and are particularly informative when plotted as concentration contour maps or downhole concentration diagrams. On Leg 2 additional core scans were made with X-ray Computed Tomography (X-ray CT) and infrared images from the visible-shortwave infrared imaging spectroscopy (IR) systems on board. XRF-CL, X-ray CT and IR imaging plots used together provide detailed information on rock compositions, textures and mineralogy that assist naked eye visual observations. Examples of some uses of XRF-CL geochemical maps and downhole data are shown. XRF-CL and IR scans of listvenite clearly show zones of magnesite, dolomite and the Cr-rich mica, fuchsite that are subdued in visual observation, and these scans can be used to calculate variations in proportions of these minerals in Hole BT1B cores. In Hole GT3A XRF-CL data can be used to distinguish compositional changes in different generations of sheeted dikes and gabbros and when combined with visual observations of intrusive relationships the detailed geochemical

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

Direct identification and analysis of heavy metals in solution (Hg, Cu, Pb, Zn, Ni) by use of in situ electrochemical X-ray fluorescence.

PubMed

O'Neil, Glen D; Newton, Mark E; Macpherson, Julie V

2015-01-01

The development and application of a new methodology, in situ electrochemical X-ray fluorescence (EC-XRF), is described that enables direct identification and quantification of heavy metals in solution. A freestanding film of boron-doped diamond serves as both an X-ray window and the electrode material. The electrode is biased at a suitable driving potential to electroplate metals from solution onto the electrode surface. Simultaneously, X-rays that pass through the back side of the electrode interrogate the time-dependent electrodeposition process by virtue of the XRF signals, which are unique to each metal. In this way it is possible to unambiguously identify which metals are in solution and relate the XRF signal intensity to a concentration of metal species in solution. To increase detection sensitivity and reduce detection times, solution is flown over the electrode surface by use of a wall-jet configuration. Initial studies focused on the in situ detection of Pb(2+), where concentration detection limits of 99 nM were established in this proof-of-concept study (although significantly lower values are anticipated with system refinement). This is more than 3 orders of magnitude lower than that achievable by XRF alone in a flowing solution (0.68 mM). In situ EC-XRF measurements were also carried out on a multimetal solution containing Hg(2+), Pb(2+), Cu(2+), Ni(2+), Zn(2+), and Fe(3+) (all at 10 μM concentration). Identification of five of these metals was possible in one simple measurement. In contrast, while anodic stripping voltammetry (ASV) also revealed five peaks, peak identification was not straightforward, requiring further experiments and prior knowledge of the metals in solution. Time-dependent EC-XRF nucleation data for the five metals, recorded simultaneously, demonstrated similar deposition rates. Studies are now underway to lower detection limits and provide a quantitative understanding of EC-XRF responses in real, multimetal solutions. Finally, the

MapX: An In Situ, Full-Frame X-Ray Spectroscopic Imager for the Biogenic Elements

NASA Technical Reports Server (NTRS)

Blake, David; Sarrazin, Philippe; Thompson, Kathy; Bristow, Thomas

2016-01-01

Microbial life exploits microscale disequilibria at boundaries where valence, chemical potential, pH, Eh, etc. vary on a length scale commensurate with the organisms themselves - tens to hundreds of micrometers. These disequilibria can exist within cracks or veins in rocks and ice, at inter- or intra-crystalline boundaries, at sediment/water or sediment/atmosphere interfaces, or even within fluid inclusions trapped inside minerals. The detection of accumulations of the biogenic elements C,N,O,P,S at appropriate concentrations on or in a mineral/ice substrate would constitute permissive evidence of extant life, but context is also required. Does the putative biosignature exist in a habitable environment? Under what conditions of P, T, and chemical potential was the host mineralogy formed? MapX is an arm-deployed contact instrument that directly images the biogenic elements C, N, O, P, S, as well as the cations of the rock-forming minerals (Na, Mg, Al, Si, K, Ca, Ti, Cr, Mn, Fe) and important anions such as Cl, Fl. The instrument provides element images having =100 micron lateral spatial resolution over a 2.5 cm X 2.5 cm area, as well as quantitative XRF spectra from ground-selected or instrument-selected Regions of Interest (ROI) on the sample. Quantitative XRF spectra from ROI can be translated into mineralogies using ground- or instrument-based algorithms. Either an X-ray tube source (X-ray fluorescence) or a radioisotope source such as 244-Cm (alpha-particle and gamma-ray fluorescence) can be used, and characteristic X-rays emitted from the sample are imaged onto an X-ray sensitive CCD through an X-ray MicroPore Optic (MPO). As a fluorescent source, 244-Cm is highly desirable in a MapX instrument intended for life detection since high-energy alpha-particles are unrivaled in fluorescence yield for the low-Z elements. The MapX design as well as baseline performance requirements for a MapX instrument intended for life detection/identification of habitable

On the distribution of uranium in hair: Non-destructive analysis using synchrotron radiation induced X-ray fluorescence microprobe techniques

NASA Astrophysics Data System (ADS)

Israelsson, A.; Eriksson, M.; Pettersson, H. B. L.

2015-06-01

In the present study the distribution of uranium in single human hair shafts has been evaluated using two synchrotron radiation (SR) based micro X-ray fluorescence techniques; SR μ-XRF and confocal SR μ-XRF. The hair shafts originated from persons that have been exposed to elevated uranium concentrations. Two different groups have been studied, i) workers at a nuclear fuel fabrication factory, exposed mainly by inhalation and ii) owners of drilled bedrock wells exposed by ingestion of water. The measurements were carried out on the FLUO beamline at the synchrotron radiation facility ANKA, Karlsruhe. The experiment was optimized to detect U with a beam size of 6.8 μm × 3 μm beam focus allowing detection down to ppb levels of U in 10 s (SR μ-XRF setup) and 70 s (SR confocal μ-XRF setup) measurements. It was found that the uranium was present in a 10-15 μm peripheral layer of the hair shafts for both groups studied. Furthermore, potential external hair contamination was studied by scanning of unwashed hair shafts from the workers. Sites of very high uranium signal were identified as particles containing uranium. Such particles, were also seen in complementary analyses using variable pressure electron microscope coupled with energy dispersive X-ray analyzer (ESEM-EDX). However, the particles were not visible in washed hair shafts. These findings can further increase the understanding of uranium excretion in hair and its potential use as a biomonitor.

X-ray fluorescence analysis of Mexican varieties of dried chili peppers II: Commercial and home-grown specimens

NASA Astrophysics Data System (ADS)

Romero-Dávila, E.; Miranda, J.; Pineda, J. C.

2015-07-01

Elemental analyses of samples of Mexican varieties of dried chili peppers were carried out using X-ray Fluorescence (XRF). Several specimens of Capsicum annuum L., Capsicum chinense, and Capsicum pubescens were analyzed and the results compared to previous studies of elemental contents in other varieties of Capsicum annuum (ancho, morita, chilpotle, guajillo, pasilla, and árbol). The first set of samples was bought packaged in markets. In the present work, the study focuses on home-grown samples of the árbol and chilpotle varieties, commercial habanero (Capsicum chinense), as well as commercial and home-grown specimens of manzano (Capsicum pubescencs). Samples were freeze dried and pelletized. XRF analyses were carried out using a spectrometer based on an Rh X-ray tube, using a Si-PIN detector. The system detection calibration was performed through the analysis of the NIST certified reference materials 1547 (peach leaves) and 1574 (tomato leaves), while accuracy was checked with the reference material 1571 (orchard leaves). Elemental contents of all elements in the new set of samples were similar to those of the first group. Nevertheless, it was found that commercial samples contain high amounts of Br, while home-grown varieties do not.

Polycapillary based μXRF station for 3D colour tomography

NASA Astrophysics Data System (ADS)

Hampai, D.; Cherepennikov, Yu. M.; Liedl, A.; Cappuccio, G.; Capitolo, E.; Iannarelli, M.; Azzutti, C.; Gladkikh, Yu. P.; Marcelli, A.; Dabagov, S. B.

2018-04-01

The "Rainbow X-Ray" (RXR) experimental station at XLab Frascati of the Frascati's National Laboratories (LNF) INFN is a dedicated station for X-ray fluorescence studies based on the use of polycapillary lenses in a confocal geometry. The flexible RXR layout allows investigating specimens of the dimensions ranging from several millimeters up to half meter and weighting up to several tens of kilograms. Compared to similar existing XRF stations, apart of the possibility for investigating large samples, the main advantage of this equipment is the detection system with two spectrometers optimized to work separately at high and at low X-ray energies. The confocal geometry combined with a 3-axes fine motion system makes possible 3D μXRF elemental tomographic acquisitions (colour tomography). At present this station in operation at high XRF energies is used for cultural heritage and geological applications. We present and discuss here the analytical performances of this experimental station pointing out the advantages in different application areas.

Portable X-ray fluorescence for the detection of POP-BFRs in waste plastics.

PubMed

Sharkey, Martin; Abdallah, Mohamed Abou-Elwafa; Drage, Daniel S; Harrad, Stuart; Berresheim, Harald

2018-05-17

The purpose of this study was to establish the efficacy of portable X-ray fluorescence (XRF) instrumentation as a screening tool for a variety of end of life plastics which may contain excess amounts of brominated flame retardants (BFRs), in compliance with European Union (EU) and United Nations Environment Programme (UNEP) legislative limits (low POP concentration limits - LPCLs). 555 samples of waste plastics were collected from eight waste and recycling sites in Ireland, including waste electrical and electronic equipment (WEEE), textiles, polyurethane foams (PUFs), and expanded polystyrene foams. Samples were screened for bromine content, in situ using a Niton™ XL3T GOLDD XRF analyser, the results of which were statistically compared to mass spectrometry (MS)-based measurements of polybrominated diphenyl ethers (PBDEs), hexabromocyclododecane (HBCDD) and tetrabromobisphenol-A (TBBP-A) concentrations in the same samples. Regression between XRF and MS for WEEE samples shows that, despite an overall favourable trend, large deviations occur for a cluster of samples indicative of other bromine-based compounds in some samples; even compensating for false-positives due to background interference from electronic components, XRF tends to over-estimate MS-determined BFR concentrations in the 100 to 10,000 mg kg -1 range. Substantial deviations were additionally found between results for PUFs, textiles and polystyrene samples, with the XRF over-estimating BFR concentrations by a factor of up to 1.9; this is likely due to matrix effects influencing XRF measurements. However, expanded (EPS) and extruded polystyrene (XPS) yielded much more reliable estimations of BFR-content due to a dominance of HBCDD in these materials. XRF proved much more reliable as a "pass/fail" screening tool for LPCL compliance (including a prospective LPCL on Deca-BDE based on REACH). Using a conservative threshold of BFR content exceeding legislative limits (710 mg kg -1 bromine

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

NASA Astrophysics Data System (ADS)

Dinelli, Enrico; Birke, Manfred; Reimann, Clemens; Demetriades, Alecos; DeVivo, Benedetto; Flight, Dee; Ladenberger, Anna; Albanese, Stefano; Cicchella, Domenico; Lima, Annamaria

2014-05-01

The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution in soil. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database, consisting of 2 x ca. 2100 samples spread evenly over 33 European countries, is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the Geological Survey of the Slovak Republic, AR analyses were carried out at ACME Labs, and XRF analyses at the Federal Institute for Geosciences and Natural Resources, Germany Element recovery by AR is very different, ranging from <1% (e.g. Na, Zr) to > 80% (e.g. Mn, P, Co). Recovery is controlled by mineralogy of the parent material, but geographic and climatic factors and the weathering history of the soils are also important. Nonetheless, even the very low recovery elements show wide ranges of variation and spatial patterns that are affected by other factors than soil parent material. For many elements soil pH have a clear influence on AR extractability: under acidic soil conditions almost all elements tend to be leached and their extractability is generally low. It progressively increases with increasing pH and is highest in the pH range 7-8. Critical is the clay content of the soil

In vivo quantification of lead in bone with a portable x-ray fluorescence system--methodology and feasibility.

PubMed

Nie, L H; Sanchez, S; Newton, K; Grodzins, L; Cleveland, R O; Weisskopf, M G

2011-02-07

This study was conducted to investigate the methodology and feasibility of developing a portable x-ray fluorescence (XRF) technology to quantify lead (Pb) in bone in vivo. A portable XRF device was set up and optimal settings of voltage, current, and filter combination for bone lead quantification were selected to achieve the lowest detection limit. The minimum radiation dose delivered to the subject was calculated by Monte Carlo simulations. An ultrasound device was used to measure soft tissue thickness to account for signal attenuation, and an alternative method to obtain soft tissue thickness from the XRF spectrum was developed and shown to be equivalent to the ultrasound measurements (intraclass correlation coefficient, ICC = 0.82). We tested the correlation of in vivo bone lead concentrations between the standard KXRF technology and the portable XRF technology. There was a significant correlation between the bone lead concentrations obtained from the standard KXRF technology and those obtained from the portable XRF technology (ICC = 0.65). The detection limit for the portable XRF device was about 8.4 ppm with 2 mm soft tissue thickness. The entrance skin dose delivered to the human subject was about 13 mSv and the total body effective dose was about 1.5 µSv and should pose minimal radiation risk. In conclusion, portable XRF technology can be used for in vivo bone lead measurement with sensitivity comparable to the KXRF technology and good correlation with KXRF measurements.

Multispectral processing of combined visible and x-ray fluorescence imagery in the Archimedes palimpsest

NASA Astrophysics Data System (ADS)

Walvoord, Derek; Bright, Allison; Easton, Roger L., Jr.

2008-02-01

The Archimedes palimpsest is one of the most significant early texts in the history of science that has survived to the present day. It includes the oldest known copies of text from seven treatises by Archimedes, along with pages from other important historical writings. In the 13th century, the original texts were erased and overwritten by a Christian prayer book, which was used in religious services probably into the 19th century. Since 2001, much of the text from treatises of Archimedes has been transcribed from images taken in reflected visible light and visible fluorescence generated by exposure of the parchment to ultraviolet light. However, these techniques do not work well on all pages of the manuscript, including the badly stained colophon, four pages of the manuscript obscured by icons painted during the first half of the 20th century, and some pages of non-Archimedes texts. Much of the text on the colophon and overpainted pages has been recovered from X-ray fluorescence (XRF) imagery. In this work, the XRF images of one of the other pages were combined with the bands of optical images to create hyperspectral image cubes and processed using standard statistical classification techniques developed for environmental remote sensing to test if this improved the recovery of the original text.

Holographic Interferometry (HI), Infrared Vision and X-Ray Fluorescence (XRF) spectroscopy for the assessment of painted wooden statues: a new integrated approach

NASA Astrophysics Data System (ADS)

Sfarra, Stefano; Ibarra-Castanedo, Clemente; Ridolfi, Stefano; Cerichelli, Giorgio; Ambrosini, Dario; Paoletti, Domenica; Maldague, Xavier

2014-06-01

Wood has been routinely employed in decorative arts, as well as in sculptures and paintings (support) during the Middle Ages, because of its unique aesthetic virtues. It may safely be assumed that wood, as a material for monumental sculpture, was much more commonly employed in the mediaeval period than existing examples would seem to indicate (Bulletin of the metropolitan Museum of Art, 2013). Wood is easily obtainable; it could be carved and put in place with less difficulty than stone, it is chemically stable when dry, and its surface offers a compatible substrate for paint application. However, the use of wood is not without pitfalls, and requires an understanding of its anisotropic and hygroscopic nature. It is also dimensionally unstable and subject to deterioration by fungi and insects. Moisture-related dimensional changes are certainly among the most challenging problems in painting conservation. With the purpose of preventing important damages, the use of non-or microdestructive testing (NDT) techniques is undoubtedly of paramount interest for painted wooden statues of great value. This work has a threefold purpose: (1) to validate the effectiveness of an integrated approach using near-infrared (NIR) reflectography, square pulse thermography (SPT), and holographic interferometry (HI) techniques for discovering old repairs and/or inclusions of foreign materials in a wooden structure, (2) to confirm and approximately date the restoration carried out by x-ray fluorescence (XRF) spectroscopy and energy-dispersive x-ray spectroscopy (EDS) (that is assembled with a scanning electron microscopy—SEM) techniques, and (3) to combine into a multidisciplinary approach two quantitative NDT results coming from optical and thermographic methods. The subject of the present study was a statue named "Virgin with her Child" (XIV century), whose origins are mysterious and not properly documented.

Identifying Objects via Encased X-Ray-Fluorescent Materials - the Bar Code Inside

NASA Technical Reports Server (NTRS)

Schramm, Harry F.; Kaiser, Bruce

2005-01-01

Systems for identifying objects by means of x-ray fluorescence (XRF) of encased labeling elements have been developed. The XRF spectra of objects so labeled would be analogous to the external bar code labels now used to track objects in everyday commerce. In conjunction with computer-based tracking systems, databases, and labeling conventions, the XRF labels could be used in essentially the same manner as that of bar codes to track inventories and to record and process commercial transactions. In addition, as summarized briefly below, embedded XRF labels could be used to verify the authenticity of products, thereby helping to deter counterfeiting and fraud. A system, as described above, is called an encased core product identification and authentication system (ECPIAS). The ECPIAS concept is a modified version of that of a related recently initiated commercial development of handheld XRF spectral scanners that would identify alloys or detect labeling elements deposited on the surfaces of objects. In contrast, an ECPIAS would utilize labeling elements encased within the objects of interest. The basic ECPIAS concept is best illustrated by means of an example of one of several potential applications: labeling of cultured pearls by labeling the seed particles implanted in oysters to grow the pearls. Each pearl farmer would be assigned a unique mixture of labeling elements that could be distinguished from the corresponding mixtures of other farmers. The mixture would be either incorporated into or applied to the surfaces of the seed prior to implantation in the oyster. If necessary, the labeled seed would be further coated to make it nontoxic to the oyster. After implantation, the growth of layers of mother of pearl on the seed would encase the XRF labels, making these labels integral, permanent parts of the pearls that could not be removed without destroying the pearls themselves. The XRF labels would be read by use of XRF scanners, the spectral data outputs of which

Evaluation of the uncertainties associated with in vivo X-ray fluorescence bone lead calibrations

NASA Astrophysics Data System (ADS)

Lodwick, Jeffrey C.

An anthropometric leg phantom developed at the University of Cincinnati (UC) was used to evaluate the effects that changes in leg position and variation between subjects has on in vivo x-ray fluorescence (XRF) measurements of stable lead in bone. The changes in leg position that were evaluated include changes in source-phantom distance ranging between 0.0 mm and 30.0 mm and phantom rotation over 40 degrees. Source-phantom distance was determined to have a significant effect on XRF measurement results particularly at source-phantom distances greater than 10.0 mm. Rotation of the leg phantom through 40 degrees was determined to have no significant effect on XRF measurement results. Between subject factors that were evaluated include bone calcium content and overlying tissue thickness. Bone calcium content was determined to have a significant effect on XRF measurements when measuring lead in micrograms per gram bone material. However, if measurement results of micrograms of lead per gram calcium (or per gram bone mineral) is used the normalization method makes the change in calcium content not significant. Overlying tissue thickness was determined to have no significant effect on XRF measurement results with tissue thickness ranging between 5.7 and 11.62 mm. The UC leg phantom was modified to include a fibula bone phantom so that the effect that the fibula has on XRF measurement results could be evaluated. The fibula was determined to have no significant effect on XRF measurement results and in the future need not be incorporated into in vivo XRF calibration phantoms. A knee phantom was also developed for purposes of calibrations of in vivo XRF measurement of lead in the patella. XRF measurement results using this phantom were compared to results of XRF measurements made using the plaster-of-Paris (POP) phantoms. A significant difference was observed between the normalized count rates of the two phantom types when either micrograms of lead per gram of bone material or

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--METALS/XRF IN DUST ANALYTICAL RESULTS

EPA Science Inventory

The Metals-XRF in Dust data set contains X-ray fluorescence (XRF) analytical results for measurements of up to 27 metals in 91 dust samples over 91 households. Samples were taken by collecting dust from the indoor floor areas in the main room and in the bedroom of the primary re...

Censoring approach to the detection limits in X-ray fluorescence analysis

NASA Astrophysics Data System (ADS)

Pajek, M.; Kubala-Kukuś, A.

2004-10-01

We demonstrate that the effect of detection limits in the X-ray fluorescence analysis (XRF), which limits the determination of very low concentrations of trace elements and results in appearance of the so-called "nondetects", can be accounted for using the statistical concept of censoring. More precisely, the results of such measurements can be viewed as the left random censored data, which can further be analyzed using the Kaplan-Meier method correcting the data for the presence of nondetects. Using this approach, the results of measured, detection limit censored concentrations can be interpreted in a nonparametric manner including the correction for the nondetects, i.e. the measurements in which the concentrations were found to be below the actual detection limits. Moreover, using the Monte Carlo simulation technique we show that by using the Kaplan-Meier approach the corrected mean concentrations for a population of the samples can be estimated within a few percent uncertainties with respect of the simulated, uncensored data. This practically means that the final uncertainties of estimated mean values are limited in fact by the number of studied samples and not by the correction procedure itself. The discussed random-left censoring approach was applied to analyze the XRF detection-limit-censored concentration measurements of trace elements in biomedical samples.

X-ray fluorescence determination of Sn, Sb, Pb in lead-based bearing alloys using a solution technique

NASA Astrophysics Data System (ADS)

Tian, Lunfu; Wang, Lili; Gao, Wei; Weng, Xiaodong; Liu, Jianhui; Zou, Deshuang; Dai, Yichun; Huang, Shuke

2018-03-01

For the quantitative analysis of the principal elements in lead-antimony-tin alloys, directly X-ray fluorescence (XRF) method using solid metal disks introduces considerable errors due to the microstructure inhomogeneity. To solve this problem, an aqueous solution XRF method is proposed for determining major amounts of Sb, Sn, Pb in lead-based bearing alloys. The alloy samples were dissolved by a mixture of nitric acid and tartaric acid to eliminated the effects of microstructure of these alloys on the XRF analysis. Rh Compton scattering was used as internal standard for Sb and Sn, and Bi was added as internal standard for Pb, to correct for matrix effects, instrumental and operational variations. High-purity lead, antimony and tin were used to prepare synthetic standards. Using these standards, calibration curves were constructed for the three elements after optimizing the spectrometer parameters. The method has been successfully applied to the analysis of lead-based bearing alloys and is more rapid than classical titration methods normally used. The determination results are consistent with certified values or those obtained by titrations.

Reevaluation of the Apollo orbital X-ray fluorescence data

NASA Technical Reports Server (NTRS)

Hubbard, N. J.; Keith, J. E.

1977-01-01

A combination of Al/Mg ratios and Al/Si ratios has provided high-quality geochemical and geological information from the Apollo orbital X-ray fluorescence data. The high sensitivity of the characteristic Si X-rays to alterations in the energy spectra of the solar X-ray flux limits the analytical usefulness of the ratios involving Si. A photometric study indicates that the Si concentration in lunar materials varies by less than about + or - 15% of the Si present. In addition, particle size and surface roughness are shown to have small effects on the characteristic fluorescent X-ray radiation of Si.

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

PubMed

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.

Polarized x-ray excitation for scatter reduction in x-ray fluorescence computed tomography.

PubMed

Vernekohl, Don; Tzoumas, Stratis; Zhao, Wei; Xing, Lei

2018-05-25

X-ray fluorescence computer tomography (XFCT) is a new molecular imaging modality which uses x-ray excitation to stimulate the emission of fluorescent photons in high atomic number contrast agents. Scatter contamination is one of the main challenges in XFCT imaging which limits the molecular sensitivity. When polarized x rays are used, it is possible to reduce the scatter contamination significantly by placing detectors perpendicular to the polarization direction. This study quantifies scatter contamination for polarized and unpolarized x-ray excitation and determines the advantages of scatter reduction. The amount of scatter in preclinical XFCT is quantified in Monte Carlo simulations. The fluorescent x rays are emitted isotropically, while scattered x rays propagate in polarization direction. The magnitude of scatter contamination is studied in XFCT simulations of a mouse phantom. In this study, the contrast agent gold is examined as an example, but a scatter reduction from polarized excitation is also expected for other elements. The scatter reduction capability is examined for different polarization intensities with a monoenergetic x-ray excitation energy of 82 keV. The study evaluates two different geometrical shapes of CZT detectors which are modeled with an energy resolution of 1 keV FWHM at an x-ray energy of 80 keV. Benefits of a detector placement perpendicular to the polarization direction are shown in iterative and analytic image reconstruction including scatter correction. The contrast to noise ratio (CNR) and the normalized mean square error (NMSE) are analyzed and compared for the reconstructed images. A substantial scatter reduction for common detector sizes was achieved for 100% and 80% linear polarization while lower polarization intensities provide a decreased scatter reduction. By placing the detector perpendicular to the polarization direction, a scatter reduction by factor up to 5.5 can be achieved for common detector sizes. The image

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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/,more » 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.« less

The Apollo 15 X-ray fluorescence experiment

NASA Technical Reports Server (NTRS)

Adler, I.

1972-01-01

The objectives of Apollo 15 X-ray fluorescence experiment were to obtain a partial chemical map of a large portion of the moon. Gamma ray and alpha particle experiments were also performed. Mapping information from approximately 150 deg east on the moon to about 50 deg west was secured. Secondary X-rays characteristic of silicon, aluminum, and magnesium were measured.

Application of portable X-ray fluorescence spectrometry in environmental investigation of heavy metal-contaminated sites and comparison with laboratory analysis

NASA Astrophysics Data System (ADS)

Ding, Liang; Wang, Shui; Cai, Bingjie; Zhang, Mancheng; Qu, Changsheng

2018-02-01

In this study, portable X-ray fluorescence spectrometry (pXRF) was used to measure the heavy metal contents of As, Cu, Cr, Ni, Pb and Zn in the soils of heavy metal-contaminated sites. The precision, accuracy and system errors of pXRF were evaluated and compared with traditional laboratory methods to examine the suitability of in situ pXRF. The results show that the pXRF analysis achieved satisfactory accuracy and precision in measuring As, Cr, Cu, Ni, Pb, and Zn in soils, and meets the requirements of the relevant detection technology specifications. For the certified reference soil samples, the pXRF results of As, Cr, Cu, Ni, Pb, and Zn show good linear relationships and coefficients of determination with the values measured using the reference analysis methods; with the exception of Ni, all the measured values were within the 95% confidence level. In the soil samples, the coefficients of determination between Cu, Zn, Pb, and Ni concentrations measured laboratory pXRF and the values measured with laboratory analysis all reach 0.9, showing a good linear relationship; however, there were large deviations between methods for Cr and As. This study provides reference data and scientific support for rapid detection of heavy metals in soils using pXRF in site investigation, which can better guide the practical application of pXRF.

EUTERPE, a small electron storage ring for XRF

NASA Astrophysics Data System (ADS)

Botman, J. I. M.; Mutsaers, P. H. A.; Hagedoorn, H. L.; De Voigt, M. J. A.

1990-04-01

A small-sized electron storage ring is under construction at the Eindhoven University of Technology which will cover the energy range of 15 to 400 MeV. At top energy the characteristic wavelength of the synchrotron radiation spectrum is 8.3 nm for the regular dipole magnets and 1.2 nm corresponding to 1.06 keV for a 10 T wiggler magnet. This will provide useful radiation for X-ray fluorescence (XRF) up to 3.2 keV. Alternatively, photon conversion with a high power CO 2 laser beam of 0.124 eV photons will generate X-rays for XRF with energies ranging from 0.5 to 300 keV, depending on the operating energy of the storage ring. This facility will provide an important extension to the activities of the Eindhoven group on PIXE, RBS and microbeam analysis. A short description of the macnine will be given together with applications and specific examples of the XRF method.

Portable TXRF Spectrometer with 10{sup -11}g Detection Limit and Portable XRF Spectromicroscope with Sub-mm Spatial Resolution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kunimura, Shinsuke; Hatakeyama, So; Sasaki, Nobuharu

A portable total reflection X-ray fluorescence (TXRF) spectrometer that we have developed is applied to trace elemental analysis of water solutions. Although a 5 W X-ray tube is used in the portable TXRF spectrometer, detection limits of several ppb are achieved for 3d transition metal elements and trace elements in a leaching solution of soils, a leaching solution of solder, and alcoholic beverages are detected. Portable X-ray fluorescence (XRF) spectromicroscopes with a 1 W X-ray tube and an 8 W X-ray tube are also presented. Using the portable XRF spectromicroscope with the 1 W X-ray tube, 93 ppm of Crmore » is detected with an about 700 {mu}m spatial resolution. Spatially resolved elemental analysis of a mug painted with blue, red, green, and white is performed using the two portable spectromicroscopes, and the difference in elemental composition at each paint is detected.« less

Trace elements in natural azurite pigments found in illuminated manuscript leaves investigated by synchrotron x-ray fluorescence and diffraction mapping

NASA Astrophysics Data System (ADS)

Smieska, Louisa M.; Mullett, Ruth; Ferri, Laurent; Woll, Arthur R.

2017-07-01

We present trace-element and composition analysis of azurite pigments in six illuminated manuscript leaves, dating from the thirteenth to sixteenth century, using synchrotron-based, large-area x-ray fluorescence (SR-XRF) and diffraction (SR-XRD) mapping. SR-XRF mapping reveals several trace elements correlated with azurite, including arsenic, zirconium, antimony, barium, and bismuth, that appear in multiple manuscripts but were not always detected by point XRF. Within some manuscript leaves, variations in the concentration of trace elements associated with azurite coincide with distinct regions of the illuminations, suggesting systematic differences in azurite preparation or purification. Variations of the trace element concentrations in azurite are greater among different manuscript leaves than the variations within each individual leaf, suggesting the possibility that such impurities reflect distinct mineralogical/geologic sources. SR-XRD maps collected simultaneously with the SR-XRF maps confirm the identification of azurite regions and are consistent with impurities found in natural mineral sources of azurite. In general, our results suggest the feasibility of using azurite trace element analysis for provenance studies of illuminated manuscript fragments, and demonstrate the value of XRF mapping in non-destructive determination of trace element concentrations within a single pigment.

[Development of X-ray excited fluorescence spectrometer].

PubMed

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.

Fluorescent x-ray computed tomography to visualize specific material distribution

NASA Astrophysics Data System (ADS)

Takeda, Tohoru; Yuasa, Tetsuya; Hoshino, Atsunori; Akiba, Masahiro; Uchida, Akira; Kazama, Masahiro; Hyodo, Kazuyuki; Dilmanian, F. Avraham; Akatsuka, Takao; Itai, Yuji

1997-10-01

Fluorescent x-ray computed tomography (FXCT) is being developed to detect non-radioactive contrast materials in living specimens. The FXCT systems consists of a silicon channel cut monochromator, an x-ray slit and a collimator for detection, a scanning table for the target organ and an x-ray detector for fluorescent x-ray and transmission x-ray. To reduce Compton scattering overlapped on the K(alpha) line, incident monochromatic x-ray was set at 37 keV. At 37 keV Monte Carlo simulation showed almost complete separation between Compton scattering and the K(alpha) line. Actual experiments revealed small contamination of Compton scattering on the K(alpha) line. A clear FXCT image of a phantom was obtained. Using this system the minimal detectable dose of iodine was 30 ng in a volume of 1 mm3, and a linear relationship was demonstrated between photon counts of fluorescent x-rays and the concentration of iodine contrast material. The use of high incident x-ray energy allows an increase in the signal to noise ratio by reducing the Compton scattering on the K(alpha) line.

Rapid limit tests for metal impurities in pharmaceutical materials by X-ray fluorescence spectroscopy using wavelet transform filtering.

PubMed

Arzhantsev, Sergey; Li, Xiang; Kauffman, John F

2011-02-01

We introduce a new method for analysis of X-ray fluorescence (XRF) spectra based on continuous wavelet transform filters, and the method is applied to the determination of toxic metals in pharmaceutical materials using hand-held XRF spectrometers. The method uses the continuous wavelet transform to filter the signal and noise components of the spectrum. We present a limit test that compares the wavelet domain signal-to-noise ratios at the energies of the elements of interest to an empirically determined signal-to-noise decision threshold. The limit test is advantageous because it does not require the user to measure calibration samples prior to measurement, though system suitability tests are still recommended. The limit test was evaluated in a collaborative study that involved five different hand-held XRF spectrometers used by multiple analysts in six separate laboratories across the United States. In total, more than 1200 measurements were performed. The detection limits estimated for arsenic, lead, mercury, and chromium were 8, 14, 20, and 150 μg/g, respectively.

Mapping Henry: Synchrotron-sourced X-ray fluorescence mapping and ultra-high-definition scanning of an early Tudor portrait of Henry VIII

NASA Astrophysics Data System (ADS)

Dredge, Paula; Ives, Simon; Howard, Daryl L.; Spiers, Kathryn M.; Yip, Andrew; Kenderdine, Sarah

2015-11-01

A portrait of Henry VIII on oak panel c. 1535 has recently undergone technical examination to inform questions regarding authorship and the painting's relationship to a group of similar works in the collections of the National Portrait Gallery, London, and the Society of Antiquaries. Due to previous conservation treatments of the painting, the conventional transmission X-radiograph image was difficult to interpret. As a result, the painting underwent high-definition X-ray fluorescence (XRF) elemental mapping on the X-ray fluorescence microscopy beamline of the Australian Synchrotron. Scans were conducted at 12.6 and 18.5 keV, below and above the lead (Pb) L edges, respectively. Typical scan parameters were 120 μm pixel size at 7 ms dwell time, with the largest scan covering an area 545 × 287 mm2 collected in 23 h (10.8 MP). XRF mapping of the panel has guided the conservation treatment of the painting and the revelation of previously obscured features. It has also provided insight into the process of making of the painting. The informative and detailed elemental maps, alongside ultra-high-definition scans of the painting undertaken before and after varnish and over-paint removal, have assisted in comparison of the finely painted details with the London paintings. The resolution offered by the combination of imaging techniques identifies pigment distribution at an extremely fine scale, enabling a new understanding of the artist's paint application.

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

NASA Astrophysics Data System (ADS)

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

2013-06-01

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

Determining the 40K radioactivity in rocks using x-ray spectrometry

NASA Astrophysics Data System (ADS)

Pilakouta, M.; Kallithrakas-Kontos, N.; Nikolaou, G.

2017-09-01

In this paper we propose an experimental method for the determination of potassium-40 (40K) radioactivity in commercial granite samples using x-ray fluorescence (XRF). The method correlates the total potassium concentration (yield) in samples deduced by XRF analysis with the radioactivity of the sample due to the 40K radionuclide. This method can be used in an undergraduate student laboratory. A brief theoretical background and description of the method, as well as some results and their interpretation, are presented.

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

PubMed

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

2010-06-01

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

Optimizing total reflection X-ray fluorescence for direct trace element quantification in proteins I: Influence of sample homogeneity and reflector type

NASA Astrophysics Data System (ADS)

Wellenreuther, G.; Fittschen, U. E. A.; Achard, M. E. S.; Faust, A.; Kreplin, X.; Meyer-Klaucke, W.

2008-12-01

Total reflection X-ray fluorescence (TXRF) is a very promising method for the direct, quick and reliable multi-elemental quantification of trace elements in protein samples. With the introduction of an internal standard consisting of two reference elements, scandium and gallium, a wide range of proteins can be analyzed, regardless of their salt content, buffer composition, additives and amino acid composition. This strategy also enables quantification of matrix effects. Two potential issues associated with drying have been considered in this study: (1) Formation of heterogeneous residues of varying thickness and/or density; and (2) separation of the internal standard and protein during drying (which has to be prevented to allow accurate quantification). These issues were investigated by microbeam X-ray fluorescence (μXRF) with special emphasis on (I) the influence of sample support and (II) the protein / buffer system used. In the first part, a model protein was studied on well established sample supports used in TXRF, PIXE and XRF (Mylar, siliconized quartz, Plexiglas and silicon). In the second part we imaged proteins of different molecular weight, oligomerization state, bound metals and solubility. A partial separation of protein and internal standard was only observed with untreated silicon, suggesting it may not be an adequate support material. Siliconized quartz proved to be the least prone to heterogeneous drying of the sample and yielded the most reliable results.

MapX An In Situ, Full-frame X-Ray Spectroscopic Imager for Planetary Science and Astrobiology

NASA Technical Reports Server (NTRS)

Blake, David; Sarrazin, Philippe; Thompson, Kathleen; Bristow, Thomas

2017-01-01

Microbial life exploits micron-scale disequilibria at boundaries where valence, chemical potential, pH, Eh, etc. vary on a length scale commensurate with the organisms - 10's to 100's of microns. The detection of accumulations of the biogenic elements C,N,O,P,S at appropriate concentrations on or in a mineral/ice substrate would constitute permissive evidence of extant life, but context is also required. Does the putative biosignature exist under habitable conditions? Under what conditions of P, T, and chemical potential was the host mineralogy formed? MapX is an in situ robotic spacecraft instrument that images the biogenic elements C, N, O, P, S, as well as the cations of the rock-forming minerals (Na, Mg, Al, Si, K, Ca, Ti, Cr, Mn, Fe) and important anions such as Cl, Fl. MapX provides element maps with less than or equal to100 microns resolution over a 2.5 cm X 2.5 cm area, as well as quantitative XRF spectra from ground- or instrument-selected Regions of Interest (ROI). XRF spectra are converted to mineralogies using ground- or instrument-based algorithms. Either X-ray tube or radioisotope sources such as 244Cm (Alpha-particle and gamma- ray fluorescence) can be used. Fluoresced sample Xrays are imaged onto an X-ray sensitive CCD through an X-ray MicroPore Optic (MPO). The MapX design as well as baseline performance requirements for a MapX instrument intended for life detection / identification of habitable environments will be presented.

Assessing arsenic and selenium in a single nail clipping using portable X-ray fluorescence.

PubMed

Fleming, David E B; Nader, Michel N; Foran, Kelly A; Groskopf, Craig; Reno, Michael C; Ware, Chris S; Tehrani, Mina; Guimarães, Diana; Parsons, Patrick J

2017-02-01

The feasibility of measuring arsenic and selenium contents in a single nail clipping was investigated using a small-focus portable X-ray fluorescence (XRF) instrument with monochromatic excitation beams. Nail clipping phantoms supplemented with arsenic and selenium to produce materials with 0, 5, 10, 15, and 20µg/g were used for calibration purposes. In total, 10 different clippings were analyzed at two different measurement positions. Energy spectra were fit with detection peaks for arsenic K α , selenium K α , arsenic K β , selenium K β , and bromine K α characteristic X-rays. Data analysis was performed under two distinct conditions of fitting constraint. Calibration lines were established from the amplitude of each of the arsenic and selenium peaks as a function of the elemental contents in the clippings. The slopes of the four calibration lines were consistent between the two conditions of analysis. The calculated minimum detection limit (MDL) of the method, when considering the K α peak only, ranged from 0.210±0.002µg/g selenium under one condition of analysis to 0.777±0.009µg/g selenium under another. Compared with previous portable XRF nail clipping studies, MDLs were substantially improved for both arsenic and selenium. The new measurement technique had the additional benefits of being short in duration (~3min) and requiring only a single nail clipping. The mass of the individual clipping used did not appear to play a major role in signal strength, but positioning of the clipping is important. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2008-02-01

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

Development of a fluorescent x-ray source for medical imaging

NASA Astrophysics Data System (ADS)

Toyofuku, F.; Tokumori, K.; Nishimura, K.; Saito, T.; Takeda, T.; Itai, Y.; Hyodo, K.; Ando, M.; Endo, M.; Naito, H.; Uyama, C.

1995-02-01

A fluorescent x-ray source for medical imaging, such as K-edge subtraction angiography and monochromatic x-ray CT, has been developed. Using a 6.5 GeV accumulation ring in Tsukuba, fluorescent x rays, which range from about 30 to 70 keV are generated by irradiating several target materials. Measurements have been made of output intensities and energy spectra for different target angles and extraction angles. The intensities of fluorescent x rays at a 30 mA beam current are on the order of 1-3×106 photons/mm2/s at 30 cm from the local spot where the incident beam is collimated to 1 mm2. A phantom which contains three different contrast media (iodine, barium, gadolinium) was used for the K-edge energy subtraction, and element selective CT images were obtained.

XRF-measured bone lead (Pb) as a biomarker for Pb exposure and toxicity among children diagnosed with Pb poisoning.

PubMed

Specht, Aaron J; Lin, Yanfen; Weisskopf, Marc; Yan, Chonghuai; Hu, Howard; Xu, Jian; Nie, Linda H

2016-01-01

Childhood lead (Pb) poisoning remains a global issue, especially in industrial areas. In this study, 115 children with average age 5.7 years were recruited as either patient diagnosed with Pb poisoning or controls at Xinhua Hospital in China. The subjects' bone Pb was measured with a K-shell X-ray fluorescence (KXRF) and a portable X-ray fluorescence (XRF) system. A significant correlation between KXRF bone Pb and blood Pb and portable XRF and KXRF measurements were observed. The half-life of blood-lead was calculated to be 9.96 ± 3.92 d. Our results indicate that bone is a useful biomarker for Pb in children.

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

NASA Astrophysics Data System (ADS)

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

1999-09-01

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

Micro-XRF complemented by x-radiography and digital microscopy imaging for the study of hidden paintings

NASA Astrophysics Data System (ADS)

Gasanova, Svetlana; Hermon, Sorin

2017-07-01

The present study describes a novel approach to the study of hidden by integrating the non-invasive micro-X-Ray Fluorescence spectroscopy, X-radiography and digital microscopy. The case study analysed is a portrait of a male figure discovered under the painting of Ecce Homo, attributed to Titian's studio with an estimated date in the 1550s. The X-radiography images exposed the details of the underpainting, which appeared to be a nearly finished portrait of a standing man, overpainted by the current composition of Ecce Homo at a 180° angle. The microscopy observations of the upper painting's cracks and flaked areas enabled the study of the exposed underlayers in terms of their colour appearance and pigment particles. The subsequent pigment analysis was performed by micro-XRF. Since the described XRF analysis was performed not in scanner mode, the correct selection of the measurement spots for the micro analysis and separation between pigments of the lower and the upper painting was of paramount importance. The described approach for spot selection was based on the results of the preceding X-radiography and digital microscopy tests. The presence of lead white, vermilion, copper green and iron earth in the underlying portrait was confirmed by the multiple point XRF analysis of Pb, Hg, Cu, Fe and Mn lines. The described investigation method proved to be useful in the identification of the pigments of the underlying painting and consequently assisted in the tentative reconstruction of its colour palette. Moreover, the undertaken approach allowed discovering the potential of micro-XRF technique in the study of hidden compositions.

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

USGS Publications Warehouse

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.

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

NASA Astrophysics Data System (ADS)

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

2004-12-01

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

X-ray fluorescence tomographic system design and image reconstruction.

PubMed

Cong, Wenxiang; Shen, Haiou; Cao, Guohua; Liu, Hong; Wang, Ge

2013-01-01

In this paper, we presented a new design of x-ray fluorescence CT imaging system. For detecting fuorescence signals of gold nanoparticles in-vivo, multiple spectroscopic detectors are arranged and rotated orthogonal to an excited region of interest so that a localized scan can be acquired with a maximized efficiency. Excitation filtration was employed to minimize the effects of low-energy x-rays and background scattering for lowering radiation dose to the object. Numerical simulations showed that the radiation dose is less than 300 mGy/second for a complete 30 views tomographic scan; and the sensitivity of 3D fluorescence signal detection is up to 0.2% contrast concentrations of nanoparticles. The x-ray fluorescence computed tomography is an important molecular imaging tool. It can be used directly in samall animal research. It has great translational potential for future clinical applications.

A novel technique to produce x-rays for XRF, medical, and scientific purposes

NASA Astrophysics Data System (ADS)

Camara, Carlos G.; Putterman, Seth J.; Kotowski, Andy

2015-08-01

A long-standing mystery in science is the process whereby charge spontaneously exchanges between different materials that are brought into contact. After thousands of years of study there is no ab initio theory of tribocharging. As such it is an area of R&D that is not yet tethered to the first principles of physics and is wide open for new inventions. In 2008, Camara et al at UCLA discovered that tribocharging in a moderate vacuum could be used to take X-ray images. Since then, we have improved the X-ray output by 6 orders of magnitude and controlled the emission for use in a commercial product. Here we present an overview of this technology for use in X-ray fluorescence and X-ray imaging.

Addition of tracers into the polypropylene in view of automatic sorting of plastic wastes using X-ray fluorescence spectrometry.

PubMed

Bezati, F; Froelich, D; Massardier, V; Maris, E

2010-04-01

This study focused on the detection of rare earth oxides, used as tracers for the identification of polymer materials, using XRF (X-ray fluorescence) spectrometry. The tests were carried out in a test system device which allows the collection of static measurements of the samples' spectrum through the use of energy dispersive X-ray fluorescence technology. A sorting process based on tracers added into the polymer matrix is proposed in order to increase sorting selectivity of polypropylene during end-of-life recycling. Tracers consist of systems formed by one or by several substances dispersed into a material, to add a selective property to it, with the aim of improving the efficiency of sorting and high speed identification. Several samples containing rare earth oxides (Y(2)O(3), CeO(2), Nd(2)O(3), Gd(2)O(3), Dy(2)O(3), Er(2)O(3) and Yb(2)O(3)) in different concentrations were prepared in order to analyse some of the parameters which can influence the detection, such as the concentration of tracers, the acquisition time and the possible overlapping among the tracers. This work shows that by using the XRF test system device, it was possible to detect 5 of the 7 tracers tested for 1min exposure time and at a concentration level of 1000ppm. These two parameters will play an important role in the development of an industrial device, which indicates the necessity of further works that needs to be conducted in order to reduce them. Copyright 2009 Elsevier Ltd. All rights reserved.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Innov-X XT400 Series (XT400) x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the XT400 analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the XT400 analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as spiked samples with certified element concentrations. Accuracy was as

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

NASA Astrophysics Data System (ADS)

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

2013-10-01

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

Application of Compton-suppressed self-induced XRF to spent nuclear fuel measurement

NASA Astrophysics Data System (ADS)

Park, Se-Hwan; Jo, Kwang Ho; Lee, Seung Kyu; Seo, Hee; Lee, Chaehun; Won, Byung-Hee; Ahn, Seong-Kyu; Ku, Jeong-Hoe

2017-11-01

Self-induced X-ray fluorescence (XRF) is a technique by which plutonium (Pu) content in spent nuclear fuel can be directly quantified. In the present work, this method successfully measured the plutonium/uranium (Pu/U) peak ratio of a pressurized water reactor (PWR)'s spent nuclear fuel at the Korea atomic energy research institute (KAERI)'s post irradiation examination facility (PIEF). In order to reduce the Compton background in the low-energy X-ray region, the Compton suppression system additionally was implemented. By use of this system, the spectrum's background level was reduced by a factor of approximately 2. This work shows that Compton-suppressed selfinduced XRF can be effectively applied to Pu accounting in spent nuclear fuel.

Using Nondestructive Portable X-ray Fluorescence Spectrometers on Stone, Ceramics, Metals, and Other Materials in Museums: Advantages and Limitations.

PubMed

Tykot, Robert H

2016-01-01

Elemental analysis is a fundamental method of analysis on archaeological materials to address their overall composition or identify the source of their geological components, yet having access to instrumentation, its often destructive nature, and the time and cost of analyses have limited the number and/or size of archaeological artifacts tested. The development of portable X-ray fluorescence (pXRF) instruments over the past decade, however, has allowed nondestructive analyses to be conducted in museums around the world, on virtually any size artifact, producing data for up to several hundred samples per day. Major issues have been raised, however, about the sensitivity, precision, and accuracy of these devices, and the limitation of performing surface analysis on potentially heterogeneous objects. The advantages and limitations of pXRF are discussed here regarding archaeological studies of obsidian, ceramics, metals, bone, and painted materials. © The Author(s) 2015.

Optimization-Based Approach for Joint X-Ray Fluorescence and Transmission Tomographic Inversion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Di, Zichao; Leyffer, Sven; Wild, Stefan M.

2016-01-01

Fluorescence tomographic reconstruction, based on the detection of photons coming from fluorescent emission, can be used for revealing the internal elemental composition of a sample. On the other hand, conventional X-ray transmission tomography can be used for reconstructing the spatial distribution of the absorption coefficient inside a sample. In this work, we integrate both X-ray fluorescence and X-ray transmission data modalities and formulate a nonlinear optimization-based approach for reconstruction of the elemental composition of a given object. This model provides a simultaneous reconstruction of both the quantitative spatial distribution of all elements and the absorption effect in the sample. Mathematicallymore » speaking, we show that compared with the single-modality inversion (i.e., the X-ray transmission or fluorescence alone), the joint inversion provides a better-posed problem, which implies a better recovery. Therefore, the challenges in X-ray fluorescence tomography arising mainly from the effects of self-absorption in the sample are partially mitigated. The use of this technique is demonstrated on the reconstruction of several synthetic samples.« less

Influence of depositional environment in fossil teeth: a micro-XRF and XAFS study

NASA Astrophysics Data System (ADS)

Zougrou, I. M.; Katsikini, M.; Pinakidou, F.; Papadopoulou, L.; Tsoukala, E.; Paloura, E. C.

2014-04-01

The formation of metal-rich phases during the fossilization of vertebrate fossil teeth, recovered from various deposition environments in northern Greece, is studied by means of synchrotron radiation X-ray fluorescence (SR-XRF) as well as Fe and Mn K edge X-ray absorption fine structure (XAFS) spectroscopy. XRF line-scans from the samples' cross-sections revealed different contamination paths for Mn and Fe. The two-dimensional XRF maps illustrate the spatial distribution of P, Ca, Mn and Fe as well as the precipitation of Fe-rich phases in cementum, dentin and dentinal tubules. Goethite, lepidocrocite and ferrihydrite were detected in the samples' cross-section by means of Fe K edge EXAFS spectroscopy. Moreover the Fe and Mn K edge EXAFS revealed the presence of vivianite and birnessite (MnO2) on the external surface of two samples.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deng, Junjing; Vine, David J.; Chen, Si

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

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

DOE PAGES

Deng, Junjing; Vine, David J.; Chen, Si; ...

2015-02-24

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

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Niton XLt 700 Series (XLt) XRF Services x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the XLt analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the XLt analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as spiked samples with certified element concentrations. Accuracy

Non-destructive Measurement of Calcium and Potassium in Apple and Pear Using Handheld X-ray Fluorescence

PubMed Central

Kalcsits, Lee A.

2016-01-01

Calcium and potassium are essential for cell signaling, 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. PMID:27092160

Some Aspects of the Wavelength Dispersive X-Ray Determination of Fluorine Content in Various Matrices

NASA Astrophysics Data System (ADS)

Boča, M.; Gurišová, V.; Šimko, F.

2017-05-01

X-ray fluorescent signals of F Kα, Na Kα, Cl Kα, K Kα, and Ta Lα were measured by WD-XRF for various fluorine-containing systems: K2TaF7, Na3AlF6, K2ZrF6, NaF, and LiF (with NaCl and wax as additional additives). The data were recorded for 41 samples (in the form of pellets prepared in the laboratory) by more than 200 scans. The analysis of the measured fluorine X-ray fluorescence intensities demonstrated that the balance between absorption and enhancement effects depends strongly on the presence and concentration of other elements in the system. The experimental intensities of X-ray fluorescent radiation of fluorine for different systems with comparable fluorine content could differ by as much as 500%.

Feasibility for direct rapid energy dispersive X-ray fluorescence (EDXRF) and scattering analysis of complex matrix liquids by partial least squares.

PubMed

Angeyo, K H; Gari, S; Mustapha, A O; Mangala, J M

2012-11-01

The greatest challenge to material characterization by XRF technique is encountered in direct trace analysis of complex matrices. We exploited partial least squares (PLS) in conjunction with energy dispersive X-ray fluorescence and scattering (EDXRFS) spectrometry to rapidly (200 s) analyze lubricating oils. The PLS-EDXRFS method affords non-invasive quality assurance (QA) analysis of complex matrix liquids as it gave optimistic results for both heavy- and low-Z metal additives. Scatter peaks may further be used for QA characterization via the light elements. Copyright © 2012 Elsevier Ltd. All rights reserved.

TOMOX : An X-rays tomographer for planetary exploration

NASA Astrophysics Data System (ADS)

Marinangeli, Lucia; Pompilio, Loredana; Chiara Tangari, Anna; Baliva, Antonio; Alvaro, Matteo; Chiara Domeneghetti, Maria; Frau, Franco; Melis, Maria Teresa; Bonanno, Giovanni; Consolata Rapisarda, Maria; Petrinca, Paolo; Menozzi, Oliva; Lasalvia, Vasco; Pirrotta, Simone

2017-04-01

The TOMOX instrument has recently been founded under the ASI DC-EOS-2014-309 call. The TOMOX objective is to acquire both X-ray fluorescence and diffraction measurements from a sample in order to: a) achieve its chemical and mineralogical composition; b) reconstruct a 3D tomography of the sample exposed surface; c) give hints regarding the sample age. Nevertheless, this technique has applicability in several disciplines other than planetary geology, especially archaeology. The word 'tomography' is nowadays used for many 3D imaging methods, not just for those based on radiographic projections, but also for a wider range of techniques that yield 3D images. Fluorescence tomography is based on the signal produced on an energy-sensitive detector, generally placed in the horizontal plane at some angle with respect to the incident beam caused by photons coming from fluorescence emission. So far, a number of setups have been designed in order to acquire X-rays fluorescence tomograms of several different sample types. The proposed instrument is based on the MARS-XRD heritage, an ultra miniaturised XRD and XRF instrument developed for the ESA ExoMars mission. The general idea of TOMOX is to distribute both sources and detectors along a moving hemispherical support around the target sample. As a result, both sources move integrally with the detectors while the sample is observed from a fixed position, thus preserving the geometry of observation. In that way, the whole sample surface is imagined and XRD and XRF measurements are acquired continuously along all the scans. We plan to irradiate the target sample with X-rays emitted from 55Fe and 109Cd radioactive sources. 55Fe and 109Cd radioisotopes are commonly used as X-ray sources for analysis of metals in soils and rocks. The excitation energies of 55Fe and 109Cd are 5.9 keV, and 22.1 and 87.9 keV, respectively. Therefore, the elemental analysis ranges are Al to Mn with K lines excited with 55Fe; Ca to Rh, with K lines

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

PubMed

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

2014-12-07

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

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

PubMed Central

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

2014-01-01

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

X-ray fluorescence spectroscopy and Monte Carlo characterization of a unique nuragic artifact (Sardinia, Italy)

NASA Astrophysics Data System (ADS)

Brunetti, Antonio; Depalmas, Anna; di Gennaro, Francesco; Serges, Alessandra; Schiavon, Nicola

2016-07-01

The chemical composition of a unique bronze artifact known as the "Cesta" ("Basket") belonging to the ancient Nuragic civilization of the Island of Sardinia, Italy has been analyzed by combining X-ray Fluorescence Spectroscopy (XRF) with Monte Carlo simulations using the XRMC code. The "Cesta" had been discovered probably in the XVIII century with the first graphic representation reported around 1761. In a later draft (dated 1764), the basket has been depicted as being carried upside-down on the shoulder of a large bronze warrior Barthélemy (1761), Pinza (1901), Winckelmann (1776) . The two pictorial representations differed only by the presence of handles in the most recent one. XRF measurements revealed that the handles of the object are composed by brass while the other parts are composed by bronze suggesting the handles as being a later addition to the original object. The artifact is covered at its surface by a fairly thick corrosion patina. In order to determine the bronze bulk composition without the need for removing the outer patina, the artifact has been modeled as a two layer object in Monte Carlo simulations.

Assessment of Occupational Exposure to Manganese and Other Metals in Welding Fumes by Portable X-ray Fluorescence Spectrometer

PubMed Central

Laohaudomchok, Wisanti; Cavallari, Jennifer M.; Fang, Shona C.; Lin, Xihong; Herrick, Robert F.; Christiani, David C.; Weisskopf, Marc G.

2011-01-01

Elemental analysis of welding fume samples can be done using several laboratory-based techniques. However, portable measurement techniques could offer several advantages. In this study, we sought to determine whether the portable X-ray fluorescence spectrometer (XRF) is suitable for analysis of five metals (manganese, iron, zinc, copper, and chromium) on 37-mm polytetrafluoroethylene filters. Using this filter fitted on a cyclone in line with a personal pump, gravimetric samples were collected from a group of boilermakers exposed to welding fumes. We assessed the assumption of uniform deposition of these metals on the filters, and the relationships between measurement results of each metal obtained from traditional laboratory-based XRF and the portable XRF. For all five metals of interest, repeated measurements with the portable XRF at the same filter area showed good consistency (reliability ratios are equal or close to 1.0 for almost all metals). The portable XRF readings taken from three different areas of each filter were not significantly different (p-values = 0.77 to 0.98). This suggested that the metal rich PM2.5 deposits uniformly on the samples collected using this gravimetric method. For comparison of the two XRFs, the results from the portable XRF were well correlated and highly predictive of those from the laboratory XRF. The Spearman correlation coefficients were from 0.325 for chromium, to 0.995 for manganese and 0.998 for iron. The mean differences as a percent of the mean laboratory XRF readings were also small (<5%) for manganese, iron, and copper. The differences were greater for zinc and chromium, which were present at very low amounts in our samples and below the limits of detection of the portable XRF for many of the samples. These five metals were moderately to strongly correlated with the total fine particle fraction on filters (Spearman ρ = 0.41 for zinc to 0.97 for iron). Such strong correlations and comparable results suggested that the

Assessment of occupational exposure to manganese and other metals in welding fumes by portable X-ray fluorescence spectrometer.

PubMed

Laohaudomchok, Wisanti; Cavallari, Jennifer M; Fang, Shona C; Lin, Xihong; Herrick, Robert F; Christiani, David C; Weisskopf, Marc G

2010-08-01

Elemental analysis of welding fume samples can be done using several laboratory-based techniques. However, portable measurement techniques could offer several advantages. In this study, we sought to determine whether the portable X-ray fluorescence spectrometer (XRF) is suitable for analysis of five metals (manganese, iron, zinc, copper, and chromium) on 37-mm polytetrafluoroethylene filters. Using this filter fitted on a cyclone in line with a personal pump, gravimetric samples were collected from a group of boilermakers exposed to welding fumes. We assessed the assumption of uniform deposition of these metals on the filters, and the relationships between measurement results of each metal obtained from traditional laboratory-based XRF and the portable XRF. For all five metals of interest, repeated measurements with the portable XRF at the same filter area showed good consistency (reliability ratios are equal or close to 1.0 for almost all metals). The portable XRF readings taken from three different areas of each filter were not significantly different (p-values = 0.77 to 0.98). This suggested that the metal rich PM(2.5) deposits uniformly on the samples collected using this gravimetric method. For comparison of the two XRFs, the results from the portable XRF were well correlated and highly predictive of those from the laboratory XRF. The Spearman correlation coefficients were from 0.325 for chromium, to 0.995 for manganese and 0.998 for iron. The mean differences as a percent of the mean laboratory XRF readings were also small (<5%) for manganese, iron, and copper. The differences were greater for zinc and chromium, which were present at very low amounts in our samples and below the limits of detection of the portable XRF for many of the samples. These five metals were moderately to strongly correlated with the total fine particle fraction on filters (Spearman rho = 0.41 for zinc to 0.97 for iron). Such strong correlations and comparable results suggested that

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butterworth, A.L.; Becker, N.; Gainsforth, Z.

2012-03-13

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

Determination of U, Th and K in bricks by gamma-ray spectrometry, X-ray fluorescence analysis and neutron activation analysis

NASA Astrophysics Data System (ADS)

Bártová, H.; Kučera, J.; Musílek, L.; Trojek, T.; Gregorová, E.

2017-11-01

Knowledge of the content of natural radionuclides in bricks can be important in some cases in dosimetry and application of ionizing radiation. Dosimetry of naturally occurring radionuclides in matter (NORM) in general is one of them, the other one, related to radiation protection, is radon exposure evaluation, and finally, it is needed for the thermoluminescence (TL) dating method. The internal dose rate inside bricks is caused mostly by contributions of the natural radionuclides 238U, 232Th, radionuclides of their decay chains, and 40K. The decay chain of 235U is usually much less important. The concentrations of 238U, 232Th and 40K were measured by various methods, namely by gamma-ray spectrometry, X-ray fluorescence analysis (XRF), and neutron activation analysis (NAA) which was used as a reference method. These methods were compared from the point of view of accuracy, limit of detection (LOD), amount of sample needed and sample handling, time demands, and instrument availability.

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

DOEpatents

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

2010-12-28

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

High-spatial-resolution nanoparticle x-ray fluorescence tomography

NASA Astrophysics Data System (ADS)

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

2016-03-01

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

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

PubMed Central

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

2014-01-01

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

Nuclear Fuel Assay through analysis of Uranium L-shell by Hybrid L-edge/XRF Densitometer using a Surrogate Material

NASA Astrophysics Data System (ADS)

Park, Seunghoon; Joung, Sungyeop; Park, Jerry AB(; ), AC(; )

2018-01-01

Assay of L-series of nuclear material solution is useful for determination of amount of nuclear materials and ratio of minor actinide in the materials. The hybrid system of energy dispersive X-ray absorption edge spectrometry, i.e. L-edge densitometry, and X-ray fluorescence spectrometry is one of the analysis methods. The hybrid L-edge/XRF densitometer can be a promising candidate for a portable and compact equipment due to advantage of using low energy X-ray beams without heavy shielding systems and liquid nitrogen cooling compared to hybrid K-edge/XRF densitometer. A prototype of the equipment was evaluated for feasibility of the nuclear material assay using a surrogate material (lead) to avoid radiation effects from nuclear materials. The uncertainty of L-edge and XRF characteristics of the sample material and volume effects was discussed in the article.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deng, Junjing; Vine, David J.; Chen, Si

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

Quantification of 2D elemental distribution maps of intermediate-thick biological sections by low energy synchrotron μ-X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Kump, P.; Vogel-Mikuš, K.

2018-05-01

Two fundamental-parameter (FP) based models for quantification of 2D elemental distribution maps of intermediate-thick biological samples by synchrotron low energy μ-X-ray fluorescence spectrometry (SR-μ-XRF) are presented and applied to the elemental analysis in experiments with monochromatic focused photon beam excitation at two low energy X-ray fluorescence beamlines—TwinMic, Elettra Sincrotrone Trieste, Italy, and ID21, ESRF, Grenoble, France. The models assume intermediate-thick biological samples composed of measured elements, the sources of the measurable spectral lines, and by the residual matrix, which affects the measured intensities through absorption. In the first model a fixed residual matrix of the sample is assumed, while in the second model the residual matrix is obtained by the iteration refinement of elemental concentrations and an adjusted residual matrix. The absorption of the incident focused beam in the biological sample at each scanned pixel position, determined from the output of a photodiode or a CCD camera, is applied as a control in the iteration procedure of quantification.

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

NASA Astrophysics Data System (ADS)

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

2014-12-01

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

In-Situ XRF Measurements in Lunar Surface Exploration Using Apollo Samples as a Standard

NASA Technical Reports Server (NTRS)

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

2011-01-01

Samples collected during the Apollo lunar surface missions were sampled and returned to Earth by astronauts with varying degrees of geological experience. The technology used in these EVAs, or extravehicular activities, included nothing more advanced than traditional terrestrial field instruments: rock hammer, scoop, claw tool, and sample bags. 40 years after Apollo, technology is being developed that will allow for a high-resolution geochemical map to be created in the field real-time. Handheld x-ray fluorescence (XRF) technology is one such technology. We use handheld XRF to enable a broad in-situ characterization of a geologic site of interest based on fairly rapid techniques that can be implemented by either an astronaut or a robotic explorer. The handheld XRF instrument we used for this study was the Innov-X Systems Delta XRF spectrometer.

Dual-detector X-ray fluorescence imaging of ancient artifacts with surface relief

PubMed Central

Smilgies, Detlef-M.; Powers, Judson A.; Bilderback, Donald H.; Thorne, Robert E.

2012-01-01

Interpretation of X-ray fluorescence images of archeological artifacts is complicated by the presence of surface relief and roughness. Using two symmetrically arranged fluorescence detectors in a back-reflection geometry, the proper X-ray fluorescence yield can be distinguished from intensity variations caused by surface topography. This technique has been applied to the study of Roman inscriptions on marble. PMID:22713888

Impact of an external radiation field on handheld XRF measurements for nuclear forensics applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Steeb, Jennifer L.; Mertz, Carol J.; Finck, Martha R.

X-ray fluorescence (XRF) is an attractive technique for nuclear forensics applications. We evaluated a handheld, portable XRF device by applying an external radiation field (10 mR/h to 17 R/h) using two types of radiography sources: a 60Co radiography camera to observe effects from high-energy gamma emissions and an 192Ir radiography camera to observe effects from several low-energy gamma (0.604, 0.468, and 0.317 MeV) and decay daughter x-ray emissions. External radiation tests proved that radiation, in general, has a significant effect on the dead time or background at dose rates over 1 R/hr for both the 192Ir and 60Co sources.

Development of Total Reflection X-ray fluorescence spectrometry quantitative methodologies for elemental characterization of building materials and their degradation products

NASA Astrophysics Data System (ADS)

García-Florentino, Cristina; Maguregui, Maite; Marguí, Eva; Torrent, Laura; Queralt, Ignasi; Madariaga, Juan Manuel

2018-05-01

In this work, a Total Reflection X-ray fluorescence (TXRF) spectrometry based quantitative methodology for elemental characterization of liquid extracts and solids belonging to old building materials and their degradation products from a building of the beginning of 20th century with a high historic cultural value in Getxo, (Basque Country, North of Spain) is proposed. This quantification strategy can be considered a faster methodology comparing to traditional Energy or Wavelength Dispersive X-ray fluorescence (ED-XRF and WD-XRF) spectrometry based methodologies or other techniques such as Inductively Coupled Plasma Mass Spectrometry (ICP-MS). In particular, two kinds of liquid extracts were analysed: (i) water soluble extracts from different mortars and (ii) acid extracts from mortars, black crusts, and calcium carbonate formations. In order to try to avoid the acid extraction step of the materials and their degradation products, it was also studied the TXRF direct measurement of the powdered solid suspensions in water. With this aim, different parameters such as the deposition volume and the measuring time were studied for each kind of samples. Depending on the quantified element, the limits of detection achieved with the TXRF quantitative methodologies for liquid extracts and solids were set around 0.01-1.2 and 2-200 mg/L respectively. The quantification of K, Ca, Ti, Mn, Fe, Zn, Rb, Sr, Sn and Pb in the liquid extracts was proved to be a faster alternative to other more classic quantification techniques (i.e. ICP-MS), accurate enough to obtain information about the composition of the acidic soluble part of the materials and their degradation products. Regarding the solid samples measured as suspensions, it was quite difficult to obtain stable and repetitive suspensions affecting in this way the accuracy of the results. To cope with this problem, correction factors based on the quantitative results obtained using ED-XRF were calculated to improve the accuracy of

High-definition X-ray fluorescence elemental mapping of paintings.

PubMed

Howard, Daryl L; de Jonge, Martin D; Lau, Deborah; Hay, David; Varcoe-Cocks, Michael; Ryan, Chris G; Kirkham, Robin; Moorhead, Gareth; Paterson, David; Thurrowgood, David

2012-04-03

A historical self-portrait painted by Sir Arthur Streeton (1867-1943) has been studied with fast-scanning X-ray fluorescence microscopy using synchrotron radiation. One of the technique's unique strengths is the ability to reveal metal distributions in the pigments of underlying brushstrokes, thus providing information critical to the interpretation of a painting. We have applied the nondestructive technique with the event-mode Maia X-ray detector, which has the capability to record elemental maps at megapixels per hour with the full X-ray fluorescence spectrum collected per pixel. The painting poses a difficult challenge to conventional X-ray analysis, because it was completely obscured with heavy brushstrokes of highly X-ray absorptive lead white paint (2PbCO(3)·Pb(OH)(2)) by the artist, making it an excellent candidate for the application of the synchrotron-based technique. The 25 megapixel elemental maps were successfully observed through the lead white paint across the 200 × 300 mm(2) scan area. The sweeping brushstrokes of the lead white overpaint contributed significant detrimental structure to the elemental maps. A corrective procedure was devised to enhance the visualization of the elemental maps by using the elastic X-ray scatter as a proxy for the lead white overpaint. We foresee the technique applied to the most demanding of culturally significant artworks where conventional analytical methods are inadequate.

Application of X-ray synchrotron microscopy instrumentation in biology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gasperini, F. M.; Pereira, G. R.; Granjeiro, J. M.

2011-07-01

X-ray micro-fluorescence imaging technique has been used as a significant tool in order to investigate minerals contents in some kinds of materials. The aim of this study was to evaluate the elemental distribution of calcium and zinc in bone substitute materials (nano-hydroxyapatite spheres) and cortical bones through X-Ray Micro-fluorescence analysis with the increment of Synchrotron Radiation in order to evaluate the characteristics of the newly formed bone and its interface, the preexisting bone and biomaterials by the arrangement of collagen fibers and its birefringence. The elemental mapping was carried out at Brazilian Synchrotron Light Laboratory, Campinas - Sao Paulo, Brazilmore » working at D09-XRF beam line. Based on this study, the results suggest that hydroxyapatite-based biomaterials are biocompatible, promote osteo-conduction and favored bone repair. (authors)« less

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

NASA Astrophysics Data System (ADS)

Py, J.; Groetz, J.-E.; Hubinois, J.-C.; Cardona, D.

2015-04-01

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

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

NASA Astrophysics Data System (ADS)

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

In-vivo analysis of the uptake process of heavy metals through maize roots by using synchrotron X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Hwang, Bae Geun; Lee, Sang Joon; Gil, Kyehwan

2016-12-01

The uptake of heavy metals by plants has been receiving much attention for crop contamination and phytoremediation. We employed synchrotron X-ray fluorescence (XRF) spectroscopy for an in-vivo analysis of heavy-metal uptake through a strand of maize root. A focused X-ray beam of 2.5 × 2.5 μm2 in physical dimensions was scanned along horizontal lines of the maize root at intervals of 3 μm at the 4B X-ray micro-diffraction beamline of the Pohang Accelerator Laboratory (PAL). Time-resolved mapping of the fluorescence intensities from multiple metallic elements in the root tissues provided information about the radial distributions of heavy-metal elements and their temporal variations. The concentrated core stream of heavy-metal elements spread radially up to roughly 500 μm, corresponding to 40 % of the root diameter. The absorption characteristics of three heavy metals, Cr, Mn and Ni, and their physiological features were analyzed. The absolute concentrations and the contents of the heavy-metal elements in the tested maize roots were quantitatively evaluated by using the calibration curve obtained from reference samples with preset concentrations. The uptake quantities of the tested heavy-metal elements are noticeably different, although their molecular weights are similar. This study should be helpful for understanding plant physiology related with heavy-metal uptake.

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Rigaku ZSX Mini II (ZSX Mini II) XRF Services x-ray fluorescence (XRF) analyzer was demon-strated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the ZSX Mini II analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the ZSX Mini II analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as spiked samples with certified element con

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

PubMed

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

2012-04-15

Multimodal imaging technique is an alternative approach to improve sensitivity of early cancer diagnosis. In this study, highly fluorescent and strong X-ray absorption coefficient gold nanoclusters (Au NCs) are synthesized as dual-modality imaging contrast agents (CAs) for fluorescent and X-ray dual-modality imaging. The experimental results show that the as-prepared Au NCs are well constructed with ultrasmall sizes, reliable fluorescent emission, high computed tomography (CT) value and fine biocompatibility. In vivo imaging results indicate that the obtained Au NCs are capable of fluorescent and X-ray enhanced imaging. Copyright © 2012 Elsevier Inc. All rights reserved.

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

DOEpatents

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

2009-04-14

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

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

DOEpatents

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

2011-04-26

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

Application of GEM-based detectors in full-field XRF imaging

NASA Astrophysics Data System (ADS)

Dąbrowski, W.; Fiutowski, T.; Frączek, P.; Koperny, S.; Lankosz, M.; Mendys, A.; Mindur, B.; Świentek, K.; Wiącek, P.; Wróbel, P. M.

2016-12-01

X-ray fluorescence spectroscopy (XRF) is a commonly used technique for non-destructive elemental analysis of cultural heritage objects. It can be applied to investigations of provenance of historical objects as well as to studies of art techniques. While the XRF analysis can be easily performed locally using standard available equipment there is a growing interest in imaging of spatial distribution of specific elements. Spatial imaging of elemental distrbutions is usually realised by scanning an object with a narrow focused X-ray excitation beam and measuring characteristic fluorescence radiation using a high energy resolution detector, usually a silicon drift detector. Such a technique, called macro-XRF imaging, is suitable for investigation of flat surfaces but it is time consuming because the spatial resolution is basically determined by the spot size of the beam. Another approach is the full-field XRF, which is based on simultaneous irradiation and imaging of large area of an object. The image of the investigated area is projected by a pinhole camera on a position-sensitive and energy dispersive detector. The infinite depth of field of the pinhole camera allows one, in principle, investigation of non-flat surfaces. One of possible detectors to be employed in full-field XRF imaging is a GEM based detector with 2-dimensional readout. In the paper we report on development of an imaging system equipped with a standard 3-stage GEM detector of 10 × 10 cm2 equipped with readout electronics based on dedicated full-custom ASICs and DAQ system. With a demonstrator system we have obtained 2-D spatial resolution of the order of 100 μm and energy resolution at a level of 20% FWHM for 5.9 keV . Limitations of such a detector due to copper fluorescence radiation excited in the copper-clad drift electrode and GEM foils is discussed and performance of the detector using chromium-clad electrodes is reported.

Measuring iron in the brain using quantitative susceptibility mapping and X-ray fluorescence imaging

PubMed Central

Zheng, Weili; Nichol, Helen; Liu, Saifeng; Cheng, Yu-Chung N.; Haacke, E. Mark

2013-01-01

Measuring iron content in the brain has important implications for a number of neurodegenerative diseases. Quantitative susceptibility mapping (QSM), derived from magnetic resonance images, has been used to measure total iron content in vivo and in post mortem brain. In this paper, we show how magnetic susceptibility from QSM correlates with total iron content measured by X-ray fluorescence (XRF) imaging and by inductively coupled plasma mass spectrometry (ICPMS). The relationship between susceptibility and ferritin iron was estimated at 1.10 ± 0.08 ppb susceptibility per μg iron/g wet tissue, similar to that of iron in fixed (frozen/thawed) cadaveric brain and previously published data from unfixed brains. We conclude that magnetic susceptibility can provide a direct and reliable quantitative measurement of iron content and that it can be used clinically at least in regions with high iron content. PMID:23591072

X-ray frequency combs from optically controlled resonance fluorescence

NASA Astrophysics Data System (ADS)

Cavaletto, Stefano M.; Harman, Zoltán; Buth, Christian; Keitel, Christoph H.

2013-12-01

An x-ray pulse-shaping scheme is put forward for imprinting an optical frequency comb onto the radiation emitted on a driven x-ray transition, thus producing an x-ray frequency comb. A four-level system is used to describe the level structure of N ions driven by narrow-bandwidth x rays, an optical auxiliary laser, and an optical frequency comb. By including many-particle enhancement of the emitted resonance fluorescence, a spectrum is predicted consisting of equally spaced narrow lines which are centered on an x-ray transition energy and separated by the same tooth spacing as the driving optical frequency comb. Given an x-ray reference frequency, our comb could be employed to determine an unknown x-ray frequency. While relying on the quality of the light fields used to drive the ensemble of ions, the model has validity at energies from the 100 eV to the keV range.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

High resolution projection X-ray microscope equipped with fluorescent X-ray analyzer and its applications

NASA Astrophysics Data System (ADS)

Minami, K.; Saito, Y.; Kai, H.; Shirota, K.; Yada, K.

2009-09-01

We have newly developed an open type fine-focus X-ray tube "TX-510" to realize a spatial resolution of 50nm and to radiate low energy characteristic X-rays for giving high absorption contrast to images of microscopic organisms. The "TX-510" employs a ZrO/W(100) Schottky emitter and an "In-Lens Field Emission Gun". The key points of the improvements are (1) reduced spherical aberration coefficient of magnetic objective lens, (2) easy and accurate focusing, (3) newly designed astigmatism compensator, (4) segmented thin film target for interchanging the target materials by electron beam shift and (5) fluorescent X-ray analysis system.

Soft tissue measurement of arsenic and selenium in an animal model using portable X-ray fluorescence

NASA Astrophysics Data System (ADS)

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.

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

PubMed Central

Cong, Wenxiang; Shen, Haiou; Wang, Ge

2011-01-01

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

A Spectacular Radio Flare from XRF 050416a at 40 Days and Implications for the Nature of X-Ray Flashes

NASA Technical Reports Server (NTRS)

Soderberg, A. M.; Nakar, E.; Cenko, S. B.; Cameron, P. B.; Frail, D. A.; Kulkarni, S. R.; Fox, D. B.; Berger, E.; Gal-Yam, A.; Moon, D-S.;

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

NASA Astrophysics Data System (ADS)

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

2012-12-01

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

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

PubMed

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

2014-11-01

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

Performance Test of the Next Generation X-Ray Beam Position Monitor System for The APS Upgrade

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, B.; Lee, S.; Westferro, F.

The Advanced Photon Source is developing its next major upgrade (APS-U) based on the multi-bend achromat lattice. Improved beam stability is critical for the upgrade and will require keeping short-time beam angle change below 0.25 µrad and long-term angle drift below 0.6 µrad. A reliable white x-ray beam diagnostic system in the front end will be a key part of the planned beam stabilization system. This system includes an x-ray beam position monitor (XBPM) based on x-ray fluorescence (XRF) from two specially designed GlidCop A-15 absorbers, a second XBPM using XRF photons from the Exit Mask, and two white beammore » intensity monitors using XRF from the photon shutter and Compton-scattered photons from the front end beryllium window or a retractable diamond film in windowless front ends. We present orbit stability data for the first XBPM used in the feedback control during user operations, as well as test data from the second XBPM and the intensity monitors. They demonstrate that the XBPM system meets APS-U beam stability requirements.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Washington, Aaron L.; Narrows, William; Christian, Jonathan H.

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.more » 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.« less

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jones, Michael W. M.; Phillips, Nicholas W.; van Riessen, Grant A.

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.

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

NASA Technical Reports Server (NTRS)

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

1991-01-01

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

X-ray fluorescence measurements of dissolved gas and cavitation

DOE PAGES

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

2016-09-28

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

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Rontec PicoTAX x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the PicoTAX analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the PicoTAX analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as spiked samples with certified element concentrations. Accuracy was assessed by c

INNOVATIVE TECHNOLOGY VERIFICATION REPORT XRF ...

EPA Pesticide Factsheets

The Oxford ED2000 x-ray fluorescence (XRF) analyzer was demonstrated under the U.S. Environmental Protection Agency (EPA) Superfund Innovative Technology Evaluation (SITE) Program. The field portion of the demonstration was conducted in January 2005 at the Kennedy Athletic, Recreational and Social Park (KARS) at Kennedy Space Center on Merritt Island, Florida. The demonstration was designed to collect reliable performance and cost data for the ED2000 analyzer and seven other commercially available XRF instruments for measuring trace elements in soil and sediment. The performance and cost data were evaluated to document the relative performance of each XRF instrument. This innovative technology verification report describes the objectives and the results of that evaluation and serves to verify the performance and cost of the ED2000 analyzer. Separate reports have been prepared for the other XRF instruments that were evaluated as part of the demonstration. The objectives of the evaluation included determining each XRF instrument’s accuracy, precision, sample throughput, and tendency for matrix effects. To fulfill these objectives, the field demonstration incorporated the analysis of 326 prepared samples of soil and sediment that contained 13 target elements. The prepared samples included blends of environmental samples from nine different sample collection sites as well as spiked samples with certified element concentrations. Accuracy was assessed by com

Correcting for surface topography in X-ray fluorescence imaging

PubMed Central

Geil, E. C.; Thorne, R. E.

2014-01-01

Samples with non-planar surfaces present challenges for X-ray fluorescence imaging analysis. Here, approximations are derived to describe the modulation of fluorescence signals by surface angles and topography, and suggestions are made for reducing this effect. A correction procedure is developed that is effective for trace element analysis of samples having a uniform matrix, and requires only a fluorescence map from a single detector. This procedure is applied to fluorescence maps from an incised gypsum tablet. PMID:25343805

PIXE and XRF Analysis of Roman Denarii

NASA Astrophysics Data System (ADS)

Fasano, Cecilia; Raddell, Mark; Manukyan, Khachatur; Stech, Edward; Wiescher, Michael

2017-09-01

A set of Roman Denarii from the republican to the imperial period (140BC-240AD) has been studied using X-ray fluorescent (XRF) scanning and proton induced x-ray emission (PIXE) techniques. XRF and PIXE are commonly used in the study of cultural heritage objects because they are nondestructive. The combination of these two methods is also unique because of the ability to penetrate the sample with a broader spectrum of depths and energies than either could achieve on its own. The coins are from a large span of Roman history and their analysis serves to follow the economic and political change of the era using the relative silver and copper contents in each sample. In addition to analyzing the samples, the study sought to compare these two common analysis techniques and to explore the use of a standard to examine any shortcomings in either of the methods. Data sets were compared and then adjusted to a calibration curve which was created from the analysis of a number of standard solutions. The concentrations of the standard solutions were confirmed using inductively coupled plasma spectroscopy. Through this we were able to assemble results which will progress the basis of understanding of PIXE and XRF techniques as well as increase the wealth of knowledge of Ancient Roman currency.

Rapid screening of heavy metals and trace elements in environmental samples using portable X-ray fluorescence spectrometer, A comparative study

PubMed Central

McComb, Jacqueline Q.; Rogers, Christian; Han, Fengxiang X.; Tchounwou, Paul B.

2014-01-01

With industrialization, great amounts of trace elements and heavy metals have been excavated and released on the surface of the earth and dissipated into the environments. Rapid screening technology for detecting major and trace elements as well as heavy metals in variety of environmental samples is most desired. The objectives of this study were to determine the detection limits, accuracy, repeatability and efficiency of a X-ray fluorescence spectrometer (Niton XRF analyzer) in comparison with the traditional analytical methods, inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma optical emission spectrometer (ICP-MS) in screening of major and trace elements of environmental samples including estuary soils and sediments, contaminated soils, and biological samples. XRF is a fast and non-destructive method in measuring the total concentration of multi--elements simultaneously. Contrary to ICP-OES and ICP-MS, XRF analyzer is characterized by the limited preparation required for solid samples, non-destructive analysis, increased total speed and high throughout, the decreased production of hazardous waste and the low running costs as well as multi-elemental determination and portability in the fields. The current comparative study demonstrates that XRF is a good rapid non-destructive method for contaminated soils, sediments and biological samples containing higher concentrations of major and trace elements. Unfortunately, XRF does not have sensitive detection limits of most major and trace elements as ICP-OES or ICP-MS but it may serve as a rapid screening tool for locating hot spots of uncontaminated field soils and sediments. PMID:25861136

Experimental investigation of a HOPG crystal fan for x-ray fluorescence molecular imaging

NASA Astrophysics Data System (ADS)

Rosentreter, Tanja; Müller, Bernhard; Schlattl, Helmut; Hoeschen, Christoph

2017-03-01

Imaging x-ray fluorescence generally generates a conflict between the best image quality or highest sensitivity and lowest possible radiation dose. Consequently many experimental studies investigating the feasibility of this molecular imaging method, deal with either monochromatic x-ray sources that are not practical in clinical environment or accept high x-ray doses in order to maintain the advantage of high sensitivity and producing high quality images. In this work we present a x-ray fluorescence imaging setup using a HOPG crystal fan construction consisting of a Bragg reflecting analyzer array together with a scatter reducing radial collimator. This method allows for the use of polychromatic x-ray tubes that are in general easily accessible in contrast to monochromatic x-ray sources such as synchrotron facilities. Moreover this energy-selecting device minimizes the amount of Compton scattered photons while simultaneously increasing the fluorescence signal yield, thus significantly reducing the signal to noise ratio. The aim is to show the feasibility of this approach by measuring the Bragg reflected Kα fluorescence signal of an object containing an iodine solution using a large area detector with moderate energy resolution. Contemplating the anisotropic energy distribution of background scattered x-rays we compare the detection sensitivity, applying two different detector angular configurations. Our results show that even for large area detectors with limited energy resolution, iodine concentrations of 0.12 % can be detected. However, the potentially large scan times and therefore high radiation dose need to be decreased in further investigations.

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

PubMed Central

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

2014-01-01

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

Medical imaging by fluorescent x-ray CT: its preliminary clinical evaluation

NASA Astrophysics Data System (ADS)

Takeda, Tohoru; Zeniya, Tsutomu; Wu, Jin; Yu, Quanwen; Lwin, Thet T.; Tsuchiya, Yoshinori; Rao, Donepudi V.; Yuasa, Tetsuya; Yashiro, Toru; Dilmanian, F. Avraham; Itai, Yuji; Akatsuka, Takao

2002-01-01

Fluorescent x-ray CT (FXCT) with synchrotron radiation (SR) is being developed to detect the very low concentration of specific elements. The endogenous iodine of the human thyroid and the non-radioactive iodine labeled BMIPP in myocardium were imaged by FXCT. FXCT system consists of a silicon (111) double crystal monochromator, an x-ray slit, a scanning table for object positioning, a fluorescent x-ray detector, and a transmission x-ray detector. Monochromatic x-ray with 37 keV energy was collimated into a pencil beam (from 1 mm to 0.025 mm). FXCT clearly imaged endogenous iodine of thyroid and iodine labeled BMIPP in myocardium, whereas transmission x-ray CT could not demonstrate iodine. The distribution of iodine was heterogeneous within thyroid cancer, and its concentration was lower than that of normal thyroid. Distribution of BMIPP in normal rat myocardium was almost homogeneous; however, reduced uptake was slightly shown in ischemic region. FXCT is a highly sensitive imaging modality to detect very low concentration of specific element and will be applied to reveal endogenous iodine distribution in thyroid and to use tracer study with various kinds of labeled material.

In Vivo Quantification of Lead in Bone with a Portable X-ray Fluorescence (XRF) System – Methodology and Feasibility

PubMed Central

Nie, LH; Sanchez, S; Newton, K; Grodzins, L; Cleveland, RO; Weisskopf, MG

2013-01-01

This study was conducted to investigate the methodology and feasibility of developing a portable XRF technology to quantify lead (Pb) in bone in vivo. A portable XRF device was set up and optimal setting of voltage, current, and filter combination for bone lead quantification were selected to achieve the lowest detection limit. The minimum radiation dose delivered to the subject was calculated by Monte Carlo simulations. An ultrasound device was used to measure soft tissue thickness to account for signal attenuation, and an alternative method to obtain soft tissue thickness from the XRF spectrum was developed and shown to be equivalent to the ultrasound measurements (Intraclass Correlation Coefficient, ICC=0.82). We tested the correlation of in vivo bone lead concentrations between the standard KXRF technology and the portable XRF technology. There was a significant correlation between the bone lead concentrations obtained from the standard KXRF technology and those obtained from the portable XRF technology (ICC=0.65). The detection limit for the portable XRF device was about 8.4 ppm with 2 mm soft tissue thickness. The entrance skin dose delivered to the human subject was about 13 mSv and the total body effective dose was about 1.5 μSv and should pose a minimal radiation risk. In conclusion, portable XRF technology can be used for in vivo bone lead measurement with sensitivity comparable to the KXRF technology and good correlation with KXRF measurements. PMID:21242629

Vacuum Attachment for XRF Scanner

NASA Technical Reports Server (NTRS)

Schramm, Harry F.; Kaiser, Bruce

2005-01-01

Vacuum apparatuses have been developed for increasing the range of elements that can be identified by use of x-ray fluorescent (XRF) scanners of the type mentioned in the two immediately preceding articles. As a consequence of the underlying physical principles, in the presence of air, such an XRF scanner is limited to analysis of chlorine and elements of greater atomic number. When the XRF scanner is operated in a vacuum, it extends the range of analysis to lower atomic numbers - even as far as aluminum and sodium. Hence, more elements will be available for use in XRF labeling of objects as discussed in the two preceding articles. The added benefits of the extended capabilities also have other uses for NASA. Detection of elements of low atomic number is of high interest to the aerospace community. High-strength aluminum alloys will be easily analyzed for composition. Silicon, a major contaminant in certain processes, will be detectable before the process is begun, possibly eliminating weld or adhesion problems. Exotic alloys will be evaluated for composition prior to being placed in service where lives depend on them. And in the less glamorous applications, such as bolts and fasteners, substandard products and counterfeit items will be evaluated at the receiving function and never allowed to enter the operation

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

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

Confocal total reflection X-ray fluorescence technology based on an elliptical monocapillary and a parallel polycapillary X-ray optics.

PubMed

Zhu, Yu; Wang, Yabing; Sun, Tianxi; Sun, Xuepeng; Zhang, Xiaoyun; Liu, Zhiguo; Li, Yufei; Zhang, Fengshou

2018-07-01

A total reflection X-ray fluorescence (TXRF) spectrometer based on an elliptical monocapillary X-ray lens (MXRL) and a parallel polycapillary X-ray lens (PPXRL) was designed. This TXRF instrument has micro focal spot, low divergence and high intensity of incident X-ray beam. The diameter of the focal spot of MXRL was 16.5 µm, and the divergence of the incident X-ray beam was 3.4 mrad. We applied this TXRF instrument to the micro analysis of a single-layer film containing Ni deposited on a Si substrate by metal vapor vacuum arc ion source. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

DOE PAGES

Obaid, Razib; Buth, Christian; Dakovski, Georgi L.; ...

2018-01-09

Here, 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.

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

NASA Astrophysics Data System (ADS)

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.

Recovery of Degraded-Beyond-Recognition 19th Century Daguerreotypes with Rapid High Dynamic Range Elemental X-ray Fluorescence Imaging of Mercury L Emission.

PubMed

Kozachuk, Madalena S; Sham, Tsun-Kong; Martin, Ronald R; Nelson, Andrew J; Coulthard, Ian; McElhone, John P

2018-06-22

A daguerreotype image, the first commercialized photographic process, is composed of silver-mercury, and often silver-mercury-gold amalgam particles on the surface of a silver-coated copper plate. Specular and diffuse reflectance of light from these image particles produces the range of gray tones that typify these 19 th century images. By mapping the mercury distribution with rapid-scanning, synchrotron-based micro-X-ray fluorescence (μ-XRF) imaging, full portraits, which to the naked eye are obscured entirely by extensive corrosion, can be retrieved in a non-invasive, non-contact, and non-destructive manner. This work furthers the chemical understanding regarding the production of these images and suggests that mercury is retained in the image particles despite surface degradation. Most importantly, μ-XRF imaging provides curators with an image recovery method for degraded daguerreotypes, even if the artifact's condition is beyond traditional conservation treatments.

Comparison of field portable measurements of ultrafine TiO2: X-ray fluorescence, laser-induced breakdown spectroscopy, and Fourier-transform infrared spectroscopy.

PubMed

LeBouf, Ryan F; Miller, Arthur L; Stipe, Christopher; Brown, Jonathan; Murphy, Nate; Stefaniak, Aleksandr B

2013-06-01

Laboratory measurements of ultrafine titanium dioxide (TiO2) particulate matter loaded on filters were made using three field portable methods (X-ray fluorescence (XRF), laser-induced breakdown spectroscopy (LIBS), and Fourier-transform infrared (FTIR) spectroscopy) to assess their potential for determining end-of-shift exposure. Ultrafine TiO2 particles were aerosolized and collected onto 37 mm polycarbonate track-etched (PCTE) filters in the range of 3 to 578 μg titanium (Ti). Limit of detection (LOD), limit of quantification (LOQ), and calibration fit were determined for each measurement method. The LOD's were 11.8, 0.032, and 108 μg Ti per filter, for XRF, LIBS, and FTIR, respectively and the LOQ's were 39.2, 0.11, and 361 μg Ti per filter, respectively. The XRF calibration curve was linear over the widest dynamic range, up to the maximum loading tested (578 μg Ti per filter). LIBS was more sensitive but, due to the sample preparation method, the highest loaded filter measurable was 252 μg Ti per filter. XRF and LIBS had good predictability measured by regressing the predicted mass to the gravimetric mass on the filter. XRF and LIBS produced overestimations of 4% and 2%, respectively, with coefficients of determination (R(2)) of 0.995 and 0.998. FTIR measurements were less dependable due to interference from the PCTE filter media and overestimated mass by 2% with an R(2) of 0.831.

Laboratory evaluation of a field-portable sealed source X-ray fluorescence spectrometer for determination of metals in air filter samples.

PubMed

Lawryk, Nicholas J; Feng, H Amy; Chen, Bean T

2009-07-01

Recent advances in field-portable X-ray fluorescence (FP XRF) spectrometer technology have made it a potentially valuable screening tool for the industrial hygienist to estimate worker exposures to airborne metals. Although recent studies have shown that FP XRF technology may be better suited for qualitative or semiquantitative analysis of airborne lead in the workplace, these studies have not extensively addressed its ability to measure other elements. This study involved a laboratory-based evaluation of a representative model FP XRF spectrometer to measure elements commonly encountered in workplace settings that may be collected on air sample filter media, including chromium, copper, iron, manganese, nickel, lead, and zinc. The evaluation included assessments of (1) response intensity with respect to location on the probe window, (2) limits of detection for five different filter media, (3) limits of detection as a function of analysis time, and (4) bias, precision, and accuracy estimates. Teflon, polyvinyl chloride, polypropylene, and mixed cellulose ester filter media all had similarly low limits of detection for the set of elements examined. Limits of detection, bias, and precision generally improved with increasing analysis time. Bias, precision, and accuracy estimates generally improved with increasing element concentration. Accuracy estimates met the National Institute for Occupational Safety and Health criterion for nearly all the element and concentration combinations. Based on these results, FP XRF spectrometry shows potential to be useful in the assessment of worker inhalation exposures to other metals in addition to lead.

Use of small volume cups in XRF analysis of treated wood retention

Treesearch

Rene Stelzer; Adam Taylor; Patricia Lebow

2017-01-01

Efforts are underway in the United States to improve the conformance of commercially-treated wood with the applicable retention standards. As part of an effort to devise a practical method for on-site assessment of within-charge retention variation, we investigated whether small-volume x-ray fluorescence (XRF) sample cups could be used with treated wood. A range of cup...

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

PubMed

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

2014-01-01

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

Combining X-Ray Fluorescence and Magnetic Techniques to Quantify Elemental Concentrations in Coral Cores from Belize

NASA Astrophysics Data System (ADS)

Goldfarb, L. A.; Kingsley, C.; Urbalejo, A. A.; Hangsterfer, A.; Gee, J. S.; Carilli, J.; Feinberg, J. M.; Mitra, R.; Bhattacharya, A.; Field, D.

2017-12-01

Caribbean coral reefs are some of the most threatened marine ecosystems in the world. Research 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. 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 is a progress and combination of two works presented at American Geophysical Union 2016 Fall Meeting; In this research, we explore the efficacy of X-Ray Fluorescence (XRF), a widely used tool in environmental studies (but generally not in corals), to estimate detrital metal content in coral cores collected from four locations near Belize, with varying degrees of impact from coastal processes. Four 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 spanning to characterize materials present in coral skeletons. We compare the results from XRF to elemental concentrations reported from solution-based ICP-MS. Furthermore, we also compare our XRF data to magnetic measurements we have made in these same coral cores. Overall, it appears that the non-destructive XRF technique is a viable supplement to the ICP-MS in determining sediment and metal content in coral cores, and may be particularly helpful for assessing resistant phases such as

Volcanic Chemostratigraphy on the Outcrop Using Field-Portable X-Ray Fluorescence: An Example from the Basaltic Flows of Hewitt's Cove, MA.

NASA Astrophysics Data System (ADS)

Wall, A. M.; Brabander, D. J.

2005-05-01

The area of Hewitt's Cove, Hingham, Massachusetts structurally represents the southern extent of the Boston Basin, and as such, provides the opportunity to identify and recognize basin-wide events. While the stratigraphy of the Boston Basin has been developed since the advent of U-Pb geochronology and formal stratigraphic facies descriptions (Socci and Smith, 2001), the stratigraphy of the Hewitt's Cove area has not been thoroughly addressed since the work of William O. Crosby in 1894 (Billings, 1976, Bailey and Bland, 2001). Hewitt's Cove consists of an andesitic basaltic flow, approximately 150 m thick, overlain by siltstone and conglomeratic sequences. Field-Portable X-Ray Fluorescence (FP-XRF) was used on fresh and weathered surfaces on the outcrop and in hand samples, and these analyses were compared with conventional laboratory XRF analyses. The in situ field-based analyses produced a reproducible chemostratigraphy that is consistent with subsequent laboratory-based analyses. These data suggest that the series of andesitic basalt flows at Hewitt's Cove are the result of compositionally different magmatic pulses. Additional analyses must be completed to determine the extent of these pulses and the extent of variation in this area before further conclusions can be made. This study particularly demonstrates the utility of using FP-XRF in igneous geologic applications.

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

NASA Astrophysics Data System (ADS)

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.

Employing a portable X-Ray fluorescence (P-XRF) analyser and GIS to identify and map heavy metal pollution in soils of a traditional bonfire site

NASA Astrophysics Data System (ADS)

Dao, Ligang; Zhang, Chaosheng; Morrison, Liam

2010-05-01

Soils in the vicinity of bonfires are recipients of metal contaminants from burning of metal-containing materials. In order to better understand the impacts of bonfires on soils, a total of 218 surface soil samples were collected from a traditional bonfire site in Galway City, Ireland. Concentrations of Cu, Pb and Zn were determined using a portable X-ray Fluorescence (P-XRF) analyser. Strong variations were observed for these metals, and several samples contained elevated Zn concentrations which exceeded the intervention threshold of the Dutch criteria (720 mg kg-1). Spatial clusters and spatial outliers were detected using the local Moran's I index and were mapped using GIS. Two clear high value spatial clusters could be observed on the upper left side and centre part of the study area for Cu, Pb and Zn. Results of variogram analyses showed high nugget-sill-ratios for Cu, Pb and Zn, indicating strong spatial variation over short distances which could be resulted from anthropogenic activities. The spatial interpolation method of ordinary kriging was applied to produce the spatial interpolation maps for Cu, Pb and Zn, and the areas with elevated concentrations were in line with historical locations of the bonfires. The hazard maps showed small parts of the study area with Zn concentrations exceeding the Dutch intervention values. In order to prevent further contamination from bonfires, it is advised that tyres and other metal-containing wastes should not be burnt. The results in this study provide useful information for management of bonfires.

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

NASA Technical Reports Server (NTRS)

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

1977-01-01

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

Wavelength dispersive analysis with the synchrotron x ray fluorescence microprobe

NASA Technical Reports Server (NTRS)

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

1993-01-01

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

Portable X-ray fluorescence spectroscopy as a rapid screening technique for analysis of TiO2 and ZnO in sunscreens.

PubMed

Bairi, Venu Gopal; Lim, Jin-Hee; Quevedo, Ivan R; Mudalige, Thilak K; Linder, Sean W

2016-02-01

This investigation reports a rapid and simple screening technique for the quantification of titanium and zinc in commercial sunscreens using portable X-ray fluorescence spectroscopy (pXRF). A highly evolved technique, inductively coupled plasma-mass spectroscopy (ICP-MS) was chosen as a comparative technique to pXRF, and a good correlation (r 2 > 0.995) with acceptable variations (≤25%) in results between both techniques was observed. Analytical figures of merit such as detection limit, quantitation limit, and linear range of the method are reported for the pXRF technique. This method has a good linearity (r 2 > 0.995) for the analysis of titanium (Ti) in the range of 0.4-14.23 wt%, and zinc (Zn) in the range of 1.0-23.90 wt%. However, most commercial sunscreens contain organic ingredients, and these ingredients are known to cause matrix effects. The development of appropriate matrix matched working standards to obtain the calibration curve was found to be a major challenge for the pXRF measurements. In this study, we have overcome the matrix effect by using metal-free commercial sunscreens as a dispersing media for the preparation of working standards. An easy extension of this unique methodology for preparing working standards in different matrices was also reported. This method is simple, rapid, and cost-effective and, in comparison to conventional techniques (e.g., ICP-MS), did not generate toxic wastes during sample analysis.

Portable X-ray fluorescence spectroscopy as a rapid screening technique for analysis of TiO2 and ZnO in sunscreens

NASA Astrophysics Data System (ADS)

Bairi, Venu Gopal; Lim, Jin-Hee; Quevedo, Ivan R.; Mudalige, Thilak K.; Linder, Sean W.

2016-02-01

This investigation reports a rapid and simple screening technique for the quantification of titanium and zinc in commercial sunscreens using portable X-ray fluorescence spectroscopy (pXRF). A highly evolved technique, inductively coupled plasma-mass spectroscopy (ICP-MS) was chosen as a comparative technique to pXRF, and a good correlation (r2 > 0.995) with acceptable variations (≤ 25%) in results between both techniques was observed. Analytical figures of merit such as detection limit, quantitation limit, and linear range of the method are reported for the pXRF technique. This method has a good linearity (r2 > 0.995) for the analysis of titanium (Ti) in the range of 0.4-14.23 wt%, and zinc (Zn) in the range of 1.0-23.90 wt%. However, most commercial sunscreens contain organic ingredients, and these ingredients are known to cause matrix effects. The development of appropriate matrix matched working standards to obtain the calibration curve was found to be a major challenge for the pXRF measurements. In this study, we have overcome the matrix effect by using metal-free commercial sunscreens as a dispersing media for the preparation of working standards. An easy extension of this unique methodology for preparing working standards in different matrices was also reported. This method is simple, rapid, and cost-effective and, in comparison to conventional techniques (e.g., ICP-MS), did not generate toxic wastes during sample analysis.

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

PubMed

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

2013-06-01

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

The Apollo 15 X-ray fluorescence experiment

NASA Technical Reports Server (NTRS)

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

1972-01-01

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

Integrated image presentation of transmission and fluorescent X-ray CT using synchrotron radiation

NASA Astrophysics Data System (ADS)

Zeniya, T.; Takeda, T.; Yu, Q.; Hasegawa, Y.; Hyodo, K.; Yuasa, T.; Hiranaka, Y.; Itai, Y.; Akatsuka, T.

2001-07-01

We have developed a computed tomography (CT) system with synchrotron radiation (SR) to detect fluorescent X-rays and transmitted X-rays simultaneously. Both SR transmission X-ray CT (SR-TXCT) and SR fluorescent X-ray CT (SR-FXCT) can describe cross-sectional images with high spatial and contrast resolutions as compared to conventional CT. TXCT gives morphological information and FXCT gives functional information of organs. So, superposed display system for SR-FXCT and SR-TXCT images has been developed for clinical diagnosis with higher reliability. Preliminary experiment with brain phantom was carried out and the superposition of both images was performed. The superposed SR-CT image gave us both functional and morphological information easily with high reliability, thus demonstrating the usefulness of this system.

The first X-ray diffraction measurements on Mars.

PubMed

Bish, David; Blake, David; Vaniman, David; Sarrazin, Philippe; Bristow, Thomas; Achilles, Cherie; Dera, Przemyslaw; Chipera, Steve; Crisp, Joy; Downs, R T; Farmer, Jack; Gailhanou, Marc; Ming, Doug; Morookian, John Michael; Morris, Richard; Morrison, Shaunna; Rampe, Elizabeth; Treiman, Allan; Yen, Albert

2014-11-01

The Mars Science Laboratory landed in Gale crater on Mars in August 2012, and the Curiosity rover then began field studies on its drive toward Mount Sharp, a central peak made of ancient sediments. CheMin is one of ten instruments on or inside the rover, all designed to provide detailed information on the rocks, soils and atmosphere in this region. CheMin is a miniaturized X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that uses transmission geometry with an energy-discriminating CCD detector. CheMin uses onboard standards for XRD and XRF calibration, and beryl:quartz mixtures constitute the primary XRD standards. Four samples have been analysed by CheMin, namely a soil sample, two samples drilled from mudstones and a sample drilled from a sandstone. Rietveld and full-pattern analysis of the XRD data reveal a complex mineralogy, with contributions from parent igneous rocks, amorphous components and several minerals relating to aqueous alteration. In particular, the mudstone samples all contain one or more phyllosilicates consistent with alteration in liquid water. In addition to quantitative mineralogy, Rietveld refinements also provide unit-cell parameters for the major phases, which can be used to infer the chemical compositions of individual minerals and, by difference, the composition of the amorphous component.

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

NASA Astrophysics Data System (ADS)

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

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

Direct rapid analysis of trace bioavailable soil macronutrients by chemometrics-assisted energy dispersive X-ray fluorescence and scattering spectrometry.

PubMed

Kaniu, M I; Angeyo, K H; Mwala, A K; Mangala, M J

2012-06-04

Precision agriculture depends on the knowledge and management of soil quality (SQ), which calls for affordable, simple and rapid but accurate analysis of bioavailable soil nutrients. Conventional SQ analysis methods are tedious and expensive. We demonstrate the utility of a new chemometrics-assisted energy dispersive X-ray fluorescence and scattering (EDXRFS) spectroscopy method we have developed for direct rapid analysis of trace 'bioavailable' macronutrients (i.e. C, N, Na, Mg, P) in soils. The method exploits, in addition to X-ray fluorescence, the scatter peaks detected from soil pellets to develop a model for SQ analysis. Spectra were acquired from soil samples held in a Teflon holder analyzed using (109)Cd isotope source EDXRF spectrometer for 200 s. Chemometric techniques namely principal component analysis (PCA), partial least squares (PLS) and artificial neural networks (ANNs) were utilized for pattern recognition based on fluorescence and Compton scatter peaks regions, and to develop multivariate quantitative calibration models based on Compton scatter peak respectively. SQ analyses were realized with high CMD (R(2)>0.9) and low SEP (0.01% for N and Na, 0.05% for C, 0.08% for Mg and 1.98 μg g(-1) for P). Comparison of predicted macronutrients with reference standards using a one-way ANOVA test showed no statistical difference at 95% confidence level. To the best of the authors' knowledge, this is the first time that an XRF method has demonstrated utility in trace analysis of macronutrients in soil or related matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

New Developments in Hard X-ray Fluorescence Microscopy for In-situ Investigations of Trace Element Distributions in Aqueous Systems of Soil Colloids

NASA Astrophysics Data System (ADS)

Gleber, Sophie-Charlotte; Weinhausen, Britta; Köster, Sarah; Ward, Jesse; Vine, David; Finney, Lydia; Vogt, Stefan

2013-10-01

The distribution, binding and release of trace elements on soil colloids determine matter transport through the soil matrix, and necessitates an aqueous environment and short length and time scales for their study. However, not many microscopy techniques allow for that. We previously showed hard x-ray fluorescence microscopy capabilities to image aqueous colloidal soil samples [1]. As this technique provides attogram sensitivity for transition elements like Cu, Zn, and other geochemically relevant trace elements at sub micrometer spatial resolution (currently down to 150 nm at 2-ID-E [2]; below 50nm at Bionanoprobe, cf. G.Woloschak et al, this volume) combined with the capability to penetrate tens of micrometer of water, it is ideally suited for imaging the elemental content of soil colloids. To address the question of binding and release processes of trace elements on the surface of soil colloids, we developed a microfluidics based XRF flow cytometer, and expanded the applied methods of hard x-ray fluorescence microscopy towards three dimensional imaging. Here, we show (a) the 2-D imaged distributions of Si, K and Fe on soil colloids of Pseudogley samples; (b) how the trace element distribution is a dynamic, pH-dependent process; and (c) x-ray tomographic applications to render the trace elemental distributions in 3-D. We conclude that the approach presented here shows the remarkable potential to image and quantitate elemental distributions from samles within their natural aqueous microenvironment, particularly important in the environmental, medical, and biological sciences.

Investigating the Defect Structures in Transparent Conducting Oxides Using X-ray and Neutron Scattering Techniques

PubMed Central

González, Gabriela B.

2012-01-01

Transparent conducting oxide (TCO) materials are implemented into a wide variety of commercial devices because they possess a unique combination of high optical transparency and high electrical conductivity. Created during the processing of the TCOs, defects within the atomic-scale structure are responsible for their desirable optical and electrical properties. Therefore, studying the defect structure is essential to a better understanding of the behavior of transparent conductors. X-ray and neutron scattering techniques are powerful tools to investigate the atomic lattice structural defects in these materials. This review paper presents some of the current developments in the study of structural defects in n-type TCOs using x-ray diffraction (XRD), neutron diffraction, extended x-ray absorption fine structure (EXAFS), pair distribution functions (PDFs), and x-ray fluorescence (XRF). PMID:28817010

Analysis of Thousands of Prehistoric Mediterranean Obsidian Artifacts Using a Nondestructive Portable X-Ray Fluorescence Spectrometer

NASA Astrophysics Data System (ADS)

Tykot, Robert

A portable, hand-held X-ray fluorescence spectrometer has been used for a decade to elementally analyze prehistoric obsidian artifacts in the Mediterranean. Nearly 400 geological obsidian samples and 7500 obsidian artifacts have been analyzed. The pXRF can distinguish all individual sources, as well as assign artifacts specifically to most subsources. For the island sources of Lipari, Pantelleria, Sardinia, and Melos, it is important to address the usage of obsidian from specific subsources due to human selection based on physical properties of the raw material and their production practices, which may have changed over time from the Early Neolithic to the Bronze Age. The analysis of 50 or more artifacts from 60 different archaeological sites allows for statistical comparison between sites, and their contexts, geographic areas (e.g. coastal/inland, highland/lowland) and distance from geological sources. The frequency of transport between island sources and mainland sites is suggestive of maritime capabilities also for the transport of domesticated animals, ceramics, and other materials. This presentation will specifically address potential limitations of the portable XRF, including non-destructive surface analysis of potentially heterogeneous materials, and limited trace element detection compared to other analytical methods, versus its highly beneficial ``package'' of analyzing great numbers of artifacts non-destructively and rapidly without needing to export them from museums and facilities in many countries.

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

NASA Astrophysics Data System (ADS)

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

2016-01-01

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

In-situ and elementally resolved determination of the thickness uniformity of multi-ply films by confocal micro XRF.

PubMed

Peng, Song; Liu, Zhiguo; Sun, Tianxi; Wang, Guangfu; Ma, Yongzhong; Ding, Xunliang

2014-08-01

Confocal micro X-ray fluorescence (CM-XRF) with quasi-monochromatic excitation based on polycapillary X-ray optics was used to measure the thickness of multi-ply films. The relative errors of measuring an Fe film with a thickness of 16.3 μm and a Cu film with a thickness of 24.5 μm were 7.3% and 0.4%, respectively. The non-destructive and in-situ measurement of the thickness and uniformity of multi-ply films of Cu, Fe and Ni on a silicon surface was performed. CM-XRF was convenient in in-situ and elementally resolved analysis of the thickness of multi-ply films without a cumbersome theoretical correction model. Copyright © 2014 Elsevier Ltd. All rights reserved.

Feasibility of an integrated X-ray instrument for Mars exobiology and geology. [Abstract only

NASA Technical Reports Server (NTRS)

Fonda, M. L.; Schwartz, D. E.; Koppel, L. N.; Franco, E. D.; Kerner, J. A.

1994-01-01

By employing an integrated X-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details relevant to the possibility of the origin and evolution of life on Mars will be acquired. An integrated combined X Ray Fluorescence/X Ray Detection (XRF/XRD) instrument has been breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for Mars Environmental Survey (MESUR) and future Mars missions. Among others, primary objectives for the exploration of Mars include: the intense study of local areas on Mars to 'establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epochs; and to establish the global chemical and physical characteristics of the Martian surface'. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment.

A new generation of x-ray spectrometry UHV instruments at the SR facilities BESSY II, ELETTRA and SOLEIL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lubeck, J., E-mail: janin.lubeck@ptb.de; Fliegauf, R.; Holfelder, I.

A novel type of ultra-high vacuum instrument for X-ray reflectometry and spectrometry-related techniques for nanoanalytics by means of synchrotron radiation (SR) has been constructed and commissioned at BESSY II. This versa-tile instrument was developed by the PTB, Germany’s national metrology institute, and includes a 9-axis manipulator that allows for an independent alignment of the samples with respect to all degrees of freedom. In addition, it integrates a rotational and translational movement of several photodiodes as well as a translational movement of a beam-geometry-defining aperture system. Thus, the new instrument enables various analytical techniques based on energy dispersive X-ray detectors suchmore » as reference-free X-Ray Fluorescence (XRF) analysis, total-reflection XRF, grazing-incidence XRF, in addition to optional X-Ray Reflectometry (XRR) measurements or polarization-dependent X-ray absorption fine structure analyses (XAFS). Samples having a size of up to (100 × 100) mm{sup 2}; can be analyzed with respect to their mass deposition, elemental, spatial or species composition. Surface contamination, nanolayer composition and thickness, depth pro-file of matrix elements or implants, nanoparticles or buried interfaces as well as molecular orientation of bonds can be accessed. Three technology transfer projects of adapted instruments have enhanced X-Ray Spectrometry (XRS) research activities within Europe at the synchrotron radiation facilities ELETTRA (IAEA) and SOLEIL (CEA/LNE-LNHB) as well as at the X-ray innovation laboratory BLiX (TU Berlin) where different laboratory sources are used. Here, smaller chamber requirements led PTB in cooperation with TU Berlin to develop a modified instrument equipped with a 7-axis manipulator: reduced freedom in the choice of experimental geometry modifications (absence of out-of-SR-plane and reference-free XRS options) has been compensated by encoder-enhanced angular accuracy for GIXRF and XRR.« less

Chemical mapping of paleontological and archeological artifacts with synchrotron X-rays.

PubMed

Bergmann, Uwe; Manning, Phillip L; Wogelius, Roy A

2012-01-01

The application of the recently developed synchrotron rapid scanning X-ray fluorescence (SRS-XRF) technique to the mapping of large objects is the focus of this review. We discuss the advantages of SRS-XRF over traditional systems and the use of other synchrotron radiation (SR) techniques to provide corroborating spectroscopic and diffraction analyses during the same analytical session. After reviewing routine techniques used to analyze precious specimens, we present several case studies that show how SR-based methods have been successfully applied in archeology and paleontology. For example, SRS-XRF imaging of a seventh-century Qur'ān palimpsest and an overpainted original opera score from Luigi Cherubini is described. We also review the recent discovery of soft-tissue residue in fossils of Archaeopteryx and an ancient reptile, as well as work that has successfully resolved the remnants of pigment in Confuciusornis sanctus, a 120-million-year-old fossil of the oldest documented bird with a fully derived avian beak.

Some aspects of analytical chemistry as applied to water quality assurance techniques for reclaimed water: The potential use of X-ray fluorescence spectrometry for automated on-line fast real-time simultaneous multi-component analysis of inorganic pollutants in reclaimed water

NASA Technical Reports Server (NTRS)

Ling, A. C.; Macpherson, L. H.; Rey, M.

1981-01-01

The potential use of isotopically excited energy dispersive X-ray fluorescence (XRF) spectrometry for automated on line fast real time (5 to 15 minutes) simultaneous multicomponent (up to 20) trace (1 to 10 parts per billion) analysis of inorganic pollutants in reclaimed water was examined. Three anionic elements (chromium 6, arsenic and selenium) were studied. The inherent lack of sensitivity of XRF spectrometry for these elements mandates use of a preconcentration technique and various methods were examined, including: several direct and indirect evaporation methods; ion exchange membranes; selective and nonselective precipitation; and complexation processes. It is shown tha XRF spectrometry itself is well suited for automated on line quality assurance, and can provide a nondestructive (and thus sample storage and repeat analysis capabilities) and particularly convenient analytical method. Further, the use of an isotopically excited energy dispersive unit (50 mCi Cd-109 source) coupled with a suitable preconcentration process can provide sufficient sensitivity to achieve the current mandated minimum levels of detection without the need for high power X-ray generating tubes.

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

DOE PAGES

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

2016-06-17

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

X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

NASA Astrophysics Data System (ADS)

Gu, B.; Mishra, B.; Miller, C.; Wang, W.; Lai, B.; Brooks, S. C.; Kemner, K. M.; Liang, L.

2014-05-01

Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied X-ray fluorescence (XRF) microprobes to directly visualize and quantify the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg contaminated freshwater system. Up to 175 μg g-1 Hg is found on suspended particles. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM), possibly as Hg-NOM-iron oxide ternary complexes. The diatom-bound Hg is mostly found on outer surfaces of the cells, suggesting passive sorption of inorganic Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, is an important sink for Hg in natural aquatic environments.

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

NASA Astrophysics Data System (ADS)

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

2016-06-01

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

Copper uptake, intracellular localization, and speciation in marine microalgae measured by synchrotron radiation X-ray fluorescence and absorption microspectroscopy

DOE PAGES

Adams, Merrin S.; Dillon, Carolyn T.; Vogt, Stefan; ...

2016-07-20

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 gmore » 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. Here, 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.« less

Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

NASA Astrophysics Data System (ADS)

Maruthi, Y. A.; Das, N. Lakshmana; Ramprasad, S.; Ram, S. S.; Sudarshan, M.

2015-08-01

The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk

Étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES)

NASA Astrophysics Data System (ADS)

Rahmani, A.; Benyaïch, F.; Bounakhla, M.; Bilal, E.; Moutte, J.; Gruffat, J. J.; Zahry, F.

2004-11-01

Dans ce travail, nous présentons une étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES). Les résultats de la calibration des spectromètres à dispersion d'énergie, à excitation par sources radioactives (55Fe, 109Cd et 241Am) et à excitation secondaire (cible secondaire Mo et Cu) du Centre National pour l'Energie, les Sciences et les Techniques Nucléaires (CNESTEN, Rabat, Maroc) sur des échantillons étalons de références de l'Agence International de l'Energie Atomique (AIEA) et du Community Bureau of Référence (BCR) ont été comparés aux résultats d'analyse des mêmes échantillons étalons par la spectrométrie X à dispersion de longueur d'onde (WD-XRF) et par spectrométrie d'émission atomique à source plasma couplé par induction (ICP-AES) au département GENERIC du centre SPIN à l'Ecole des Mines de Saint-Etienne (France). Les trois techniques d'analyse utilisées donnent des résultats comparables pour le dosage des éléments majeurs, alors que pour les traces on note des déviations importantes à cause des effets de matrice qui sont difficiles à corriger dans le cas de la fluorescence X.

An Integrated XRF/XRD Instrument for Mars Exobiology and Geology Experiments

NASA Technical Reports Server (NTRS)

Koppel, L. N.; Franco, E. D.; Kerner, J. A.; Fonda, M. L.; Schwartz, D. E.; Marshall, J. R.

1993-01-01

By employing an integrated x-ray instrument on a future Mars mission, data obtained will greatly augment those returned by Viking; details characterizing the past and present environment on Mars and those relevant to the possibility of the origin and evolution of life will be acquired. A combined x-ray fluorescence/x-ray diffraction (XRF/XRD) instrument was breadboarded and demonstrated to accommodate important exobiology and geology experiment objectives outlined for MESUR and future Mars missions. Among others, primary objectives for the exploration of Mars include the intense study of local areas on Mars to establish the chemical, mineralogical, and petrological character of different components of the surface material; to determine the distribution, abundance, and sources and sinks of volatile materials, including an assessment of the biologic potential, now and during past epoches; and to establish the global chemical and physical characteristics of the Martian surface. The XRF/XRD breadboard instrument identifies and quantifies soil surface elemental, mineralogical, and petrological characteristics and acquires data necessary to address questions on volatile abundance and distribution. Additionally, the breadboard is able to characterize the biogenic element constituents of soil samples providing information on the biologic potential of the Mars environment. Preliminary breadboard experiments confirmed the fundamental instrument design approach and measurement performance.

Submicron hard X-ray fluorescence imaging of synthetic elements.

PubMed

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

2012-04-13

Synchrotron-based X-ray fluorescence microscopy (XFM) using hard X-rays focused into sub-micron spots is a powerful technique for elemental quantification and mapping, as well as microspectroscopic measurements such as μ-XANES (X-ray absorption near edge structure). We have used XFM to image and simultaneously quantify the transuranic element plutonium at the L(3) or L(2)-edge as well as Th and lighter biologically essential elements in individual rat pheochromocytoma (PC12) cells after exposure to the long-lived plutonium isotope (242)Pu. Elemental maps demonstrate that plutonium localizes principally in the cytoplasm of the cells and avoids the cell nucleus, which is marked by the highest concentrations of phosphorus and zinc, under the conditions of our experiments. The minimum detection limit under typical acquisition conditions with an incident X-ray energy of 18 keV for an average 202 μm(2) cell is 1.4 fg Pu or 2.9×10(-20) moles Pu μm(-2), which is similar to the detection limit of K-edge XFM of transition metals at 10 keV. Copper electron microscopy grids were used to avoid interference from gold X-ray emissions, but traces of strontium present in naturally occurring calcium can still interfere with plutonium detection using its L(α) X-ray emission. Copyright © 2012 Elsevier B.V. All rights reserved.

A con-focal setup for micro-XRF experiments using diamond anvil cells

NASA Astrophysics Data System (ADS)

Wilke, Max; Rickers, Karen; Vincze, Laszlo; Schmidt, Christian; Borchert, Manuela; Pascarelli, Sakura

2010-05-01

In this contribution we introduce an experimental setup to perform con-focal micro X-ray fluorescence measurements in situ in samples at high temperatures and pressures in diamond anvil cells (DAC) (e.g. Schmidt et al. 2007). The con-focal arrangement is used to suppress the background in X-ray fluorescence (XRF) spectra that stems from elastic and inelastic scattering of the diamond anvils. The setup is based on a focusing optic in the incident beam that reaches a spot of 5-10 μm and a focusing poly-capillary in front of an energy-dispersive solid-state detector. The detector poly-capillary is designed to work at a very long working distance of 50 mm in order to collect the radiation from the center of the DAC at 90° to the incident beam. The probing volume is defined by the two foci and has a size of ca. 300 μm at 8 keV and 150 μm at 19 keV as measured by scans through thin metal foils. Comparison of XRF spectra acquired with a usual detector collimator and spectra recorded with the detector capillary shows a strong suppression of XRF signal generated outside the probed volume, i.e. XRF from the gasket material and signal from elastic and Compton scattering by the diamond anvils. The ratio of the Zr K-alpha fluorescence peak to the peak of the Compton scattering changes from 0.5 (collimator) to 1.26 (detector capillary) for a ca. 1000 ppm Zr standard solution and an incident beam energy of 20 keV. For a standard solution containing ca. 1000 ppm Hf, the ratio of the L-alpha to the Compton signal increases to 6 using the detector capillary and an incident beam energy of 9.7 keV. Thus, the con-focal setup substantially improves the fluorescence to background ratio. This will result in higher sensitivities for dilute elements in the sample chamber of the DAC. Furthermore, the possibilities of interference of the sample's signal with signal from the sample environment are greatly reduced. In a broader sense, the setup can also be applied to other confined samples

Confirmation of the E(sup src)(sub Peak)-E(sub iso) (Amati) relation from the x-ray flash XRF 050416A observed by the Swift burst alert telescope

NASA Technical Reports Server (NTRS)

Sakamoti, T.; Barbier, L.; Barthelmy, S. D.; Cummings, J. R.; Fenimore, E. E.; Gehrels, N.; Hullinger, D.; Krimm, H. A.; Markwardt, C. B.

2006-01-01

We report Swift Burst Alert Telescope (BAT) observations of the X-ray flash (XRF) XRF 050416A. The fluence ratio between the 15-25 and 25-50 keV energy bands of this event is 1.5, thus making it the softest gamma-ray burst (GRB) observed by BAT so far. The spectrum is well fitted by a Band function with E(sup obs)(sub peak) of 15.0(sup +2.3)(sub -2.7) keV. Assuming the redshift of the host galaxy (z = 0.6535), the isotropic equivalent radiated energy E(sub iso) and the peak energy at the GRB rest frame (E(sup src)(sub peak)) of XRF 050416A are not only consistent with the correlation found by Amati et al. and extended to XRFs by Sakamoto et al. but also fill in the gap of this relation around the 30-80 keV range of E(sup src)(sub peak). This result tightens the validity of the E(sup src)(sub Peak)-E(sup src)(sub peak) relation from XRFs to GRBs. We also find that the jet break time estimated using the empirical relation between E(sup src)(sub peak) and the collimation corrected energy E(sub gamma), is inconsistent with the afterglow observation by the Swift X-Ray Telescope. This could be due to the extra external shock emission overlaid around the jet break time or to the nonexistence of a jet break feature for XRFs, which might be a further challenge for GRB jet emission models and XRF/GRB unification scenarios.

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

NASA Technical Reports Server (NTRS)

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

2005-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2010-01-01

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

Comparison of PIXE and XRF analysis of airborne particulate matter samples collected on Teflon and quartz fibre filters

NASA Astrophysics Data System (ADS)

Chiari, M.; Yubero, E.; Calzolai, G.; Lucarelli, F.; Crespo, J.; Galindo, N.; Nicolás, J. F.; Giannoni, M.; Nava, S.

2018-02-01

Within the framework of research projects focusing on the sampling and analysis of airborne particulate matter, Particle Induced X-ray Emission (PIXE) and Energy Dispersive X-ray Fluorescence (ED-XRF) techniques are routinely used in many laboratories throughout the world to determine the elemental concentration of the particulate matter samples. In this work an inter-laboratory comparison of the results obtained from analysing several samples (collected on both Teflon and quartz fibre filters) using both techniques is presented. The samples were analysed by PIXE (in Florence, at the 3 MV Tandetron accelerator of INFN-LABEC laboratory) and by XRF (in Elche, using the ARL Quant'X EDXRF spectrometer with specific conditions optimized for specific groups of elements). The results from the two sets of measurements are in good agreement for all the analysed samples, thus validating the use of the ARL Quant'X EDXRF spectrometer and the selected measurement protocol for the analysis of aerosol samples. Moreover, thanks to the comparison of PIXE and XRF results on Teflon and quartz fibre filters, possible self-absorption effects due to the penetration of the aerosol particles inside the quartz fibre-filters were quantified.

Nanoparticle characterization by means of scanning free grazing emission X-ray fluorescence

NASA Astrophysics Data System (ADS)

Kayser, Yves; Sá, Jacinto; Szlachetko, Jakub

2015-05-01

Nanoparticles are considered for applications in domains as various as medical and pharmaceutical sciences, opto- and microelectronics, catalysis, photovoltaics, spintronics or nano- and biotechnology. The applications realized with nanocrystals depend strongly on the physical dimensions (shape and size) and elemental constitution. We demonstrate here that grazing emission X-ray fluorescence (GEXRF) is an element sensitive technique that presents the potential for a reliable and accurate determination of the morphology of nanoparticles deposited on a flat substrate (ready-to-use devices). Thanks to the scanning-free approach of the used GEXRF setup, the composition, shape and average size of nanoparticles are determined in short time intervals, minimizing the exposure to radiation. The (scanning-free) GEXRF technique allows for in situ investigations of the nanoparticulate systems thanks to the penetration properties of both the probe X-ray beam and the emitted X-ray fluorescence signal.

Characterization of As-polluted soils by laboratory X-ray-based techniques coupled with sequential extractions and electron microscopy: the case of Crocette gold mine in the Monte Rosa mining district (Italy).

PubMed

Allegretta, Ignazio; Porfido, Carlo; Martin, Maria; Barberis, Elisabetta; Terzano, Roberto; Spagnuolo, Matteo

2018-06-24

Arsenic concentration and distribution were studied by combining laboratory X-ray-based techniques (wavelength dispersive X-ray fluorescence (WDXRF), micro X-ray fluorescence (μXRF), and X-ray powder diffraction (XRPD)), field emission scanning electron microscopy equipped with microanalysis (FE-SEM-EDX), and sequential extraction procedure (SEP) coupled to total reflection X-ray fluorescence (TXRF) analysis. This approach was applied to three contaminated soils and one mine tailing collected near the gold extraction plant at the Crocette gold mine (Macugnaga, VB) in the Monte Rosa mining district (Piedmont, Italy). Arsenic (As) concentration, measured with WDXRF, ranged from 145 to 40,200 mg/kg. XRPD analysis evidenced the presence of jarosite and the absence of any As-bearing mineral, suggesting a high weathering grade and strong oxidative conditions. However, small domains of Fe arsenate were identified by combining μXRF with FE-SEM-EDX. SEP results revealed that As was mainly associated to amorphous Fe oxides/hydroxides or hydroxysulfates (50-80%) and the combination of XRPD and FE-SEM-EDX suggested that this phase could be attributed to schwertmannite. On the basis of the reported results, As is scarcely mobile, even if a consistent As fraction (1-3 g As/kg of soil) is still potentially mobilizable. In general, the proposed combination of laboratory X-ray techniques could be successfully employed to unravel environmental issues related to metal(loid) pollution in soil and sediments.

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

PubMed

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.

Tin accumulation in spermatozoa of the rats exposed to tributyltin chloride by synchrotron radiation X-ray fluorescence (SR-XRF) analysis with microprobe

NASA Astrophysics Data System (ADS)

Homma-Takeda, S.; Nishimura, Y.; Terada, Y.; Ueno, S.; Watanabe, Y.; Yukawa, M.

2005-04-01

Organotin compounds are widely used in industry and its environmental contamination by these compounds has recently become a concern. It is known that they act as endocrine disruptors but details of the dynamics of Sn in reproductive organs are still unknown. In the present study, we attempted to determine Sn distribution in the testis of rats exposed to tributyltin chloride (TBTC) by inductively coupled argon plasma-mass spectrometry (ICP-MS) for microdissectioned seminiferous tubules and cell-selective metal determination of synchrotron radiation X-ray florescence (SR-XRF) analysis. TBTC was orally administered to rats at a dose of 45 μmol/kg per day for 3 days. One day later, Sn was detected in the microdissectioned seminiferous tubules at a level approximately equivalent to that in the testis. Significant stage-specificity of Sn accumulation was not observed in the experimental model. Sn was also detected in spermatozoa at the stage VIII seminiferous tubule, which are the final step of spermatogenesis in the testis. These data indicate that Sn accumulates in germ cells as well as in spermatozoa in a short period of TBTC exposure.

Illustration of compositional variations over time of Chinese porcelain glazes combining micro-X-ray Fluorescence spectrometry, multivariate data analysis and Seger formulas

NASA Astrophysics Data System (ADS)

Van Pevenage, J.; Verhaeven, E.; Vekemans, B.; Lauwers, D.; Herremans, D.; De Clercq, W.; Vincze, L.; Moens, L.; Vandenabeele, P.

2015-01-01

In this research, the transparent glaze layers of Chinese porcelain samples were investigated. Depending on the production period, these samples can be divided into two groups: the samples of group A dating from the Kangxi period (1661-1722), and the samples of group B produced under emperor Qianlong (1735-1795). Due to the specific sample preparation method and the small spot size of the X-ray beam, investigation of the transparent glaze layers is enabled. Despite the many existing research papers about glaze investigations of ceramics and/or porcelain ware, this research reveals new insights into the glaze composition and structure of Chinese porcelain samples. In this paper it is demonstrated, using micro-X-ray Fluorescence (μ-XRF) spectrometry, multivariate data analysis and statistical analysis (Hotelling's T-Square test) that the transparent glaze layers of the samples of groups A and B are significantly different (95% confidence level). Calculation of the Seger formulas, enabled classification of the glazes. Combining all the information, the difference in composition of the Chinese porcelain glazes of the Kangxi period and the Qianlong period can be demonstrated.

X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

NASA Astrophysics Data System (ADS)

Gu, B.; Mishra, B.; Miller, C.; Wang, W.; Lai, B.; Brooks, S. C.; Kemner, K. M.; Liang, L.

2014-09-01

Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied a synchrotron-based X-ray fluorescence (XRF) microprobe to visualize and quantify directly the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg-contaminated freshwater system. Up to 175 μg g-1 Hg is found on suspended particles, but less than 0.01% is in the form of methylmercury. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM). The diatom-bound Hg is mostly found on outer surfaces of the cells, suggesting passive sorption of Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, may play an important role in affecting the partitioning, reactivity, and biogeochemical cycling of Hg in natural aquatic environments.

X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

DOE PAGES

Gu, Baohua; Mishra, Bhoopesh; Miller, Carrie L.; ...

2014-01-01

Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied a synchrotron-based X-ray fluorescence (XRF) microprobe to visualize and quantify directly the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg-contaminated freshwater system. Up to 175 μg g −1 Hg is found on suspended particles, but less than 0.01% is in the form of methylmercury. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM). The diatom-bound Hg is mostlymore » found on outer surfaces of the cells, suggesting passive sorption of Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, may play an important role in affecting the partitioning, reactivity, and biogeochemical cycling of Hg in natural aquatic environments.« less

Determination of fluorine by total reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Tarsoly, G.; Óvári, M.; Záray, Gy.

2010-04-01

There is a growing interest in determination of low Z elements, i.e. carbon to phosphorus, in various samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as a suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). In this study, the analytical performance of the total reflection X-ray fluorescence spectrometry for determination of fluorine was investigated applying a spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a silicon drift detector (SDD) with ultra thin window was used. The detection limit for fluorine was found to be 5 mg L - 1 (equivalent to 10 ng absolute) in aqueous matrix. The linear range of the fluorine determination is between 15 and 500 mg L - 1 , within this range the precision is below 10%. The matrix effects of the other halogens (chlorine, bromine and iodine), and sulfate were also investigated. It has been established that the upper allowed concentration limit of the above interfering elements is 100, 200, 50 and 100 mg L - 1 for Cl, Br, I and sulfate, respectively. Moreover, the role of the pre-siliconization of the quartz carrier plate was investigated. It was found, that the presence of the silicone results in poorer analytical performance, which can be explained by the thicker sample residue and stronger self-absorption of the fluorescent radiation.

Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maruthi, Y. A., E-mail: ymjournal2014@gmail.com; Das, N. Lakshmana, E-mail: nldas9@gmail.com; Ramprasad, S., E-mail: ramprasadsurakala@gmail.com

The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders.more » This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk.« less

On the viability of exploiting L-shell fluorescence for X-ray polarimetry

NASA Technical Reports Server (NTRS)

Weisskopf, M. C.; Sutherland, P. G.; Elsner, R. F.; Ramsey, B. D.

1985-01-01

It has been suggested that one may build an X-ray polarimeter by exploiting the polarization dependence of the angular distribution of L-shell fluorescence photons. In this paper the sensitivity of this approach to polarimetry is examined theoretically. The calculations are applied to several detection schemes using imaging proportional counters that would have direct application in X-ray astronomy. It is found, however, that the sensitivity of this method for measuring X-ray polarization is too low to be of use for other than laboratory applications.

XRF inductive bead fusion and PLC based control system

NASA Astrophysics Data System (ADS)

Zhu, Jin-hong; Wang, Ying-jie; Shi, Hong-xin; Chen, Qing-ling; Chen, Yu-xi

2009-03-01

In order to ensure high-quality X-ray fluorescence spectrometry (XRF) analysis, an inductive bead fusion machine was developed. The prototype consists of super-audio IGBT induction heating power supply, rotation and swing mechanisms, and programmable logic controller (PLC). The system can realize sequence control, mechanical movement control, output current and temperature control. Experimental results show that the power supply can operate at an ideal quasi-resonant state, in which the expected power output and the required temperature can be achieved for rapid heating and the uniform formation of glass beads respectively.

Characterization of aluminum nitride based films with high resolution X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Anagnostopoulos, D. F.; Siozios, A.; Patsalas, P.

2018-02-01

X-ray fluorescence spectra of Al based films are measured, using a lab-scale wavelength dispersive flat crystal spectrometer. Various structures of AlN films were studied, like single layered, capped, stratified, nanostructured, crystalline, or amorphous. By optimizing the set-up for enhanced energy resolution and detection efficiency, the measured line shapes of Κα, Kβ, and KLL radiative Auger transitions are shown to be adequately detailed to allow chemical characterization. The chemistry identification is based on the pattern comparison of the emitted line shape from the chemically unknown film and the reference line shapes from standard materials, recorded under identical experimental conditions. The ultimate strength of lab-scale high resolution X-ray fluorescence spectroscopy on film analysis is verified, in cases that ordinary applied techniques like X-ray photoelectron and X-ray diffraction fail, while the characterization refers to the non-destructive determination of the bulk properties of the film and not to its surface, as the probed depth is in the micrometer range.

X-ray physico-chemical imaging during activation of cobalt-based Fischer-Tropsch synthesis catalysts

NASA Astrophysics Data System (ADS)

Beale, Andrew M.; Jacques, Simon D. M.; Di Michiel, Marco; Mosselmans, J. Frederick W.; Price, Stephen W. T.; Senecal, Pierre; Vamvakeros, Antonios; Paterson, James

2017-11-01

The imaging of catalysts and other functional materials under reaction conditions has advanced significantly in recent years. The combination of the computed tomography (CT) approach with methods such as X-ray diffraction (XRD), X-ray fluorescence (XRF) and X-ray absorption near-edge spectroscopy (XANES) now enables local chemical and physical state information to be extracted from within the interiors of intact materials which are, by accident or design, inhomogeneous. In this work, we follow the phase evolution during the initial reduction step(s) to form Co metal, for Co-containing particles employed as Fischer-Tropsch synthesis (FTS) catalysts; firstly, working at small length scales (approx. micrometre spatial resolution), a combination of sample size and density allows for transmission of comparatively low energy signals enabling the recording of `multimodal' tomography, i.e. simultaneous XRF-CT, XANES-CT and XRD-CT. Subsequently, we show high-energy XRD-CT can be employed to reveal extent of reduction and uniformity of crystallite size on millimetre-sized TiO2 trilobes. In both studies, the CoO phase is seen to persist or else evolve under particular operating conditions and we speculate as to why this is observed. This article is part of a discussion meeting issue 'Providing sustainable catalytic solutions for a rapidly changing world'.

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

PubMed

Buddhachat, Kittisak; Klinhom, Sarisa; Siengdee, Puntita; Brown, Janine L; Nomsiri, Raksiri; Kaewmong, Patcharaporn; Thitaram, Chatchote; Mahakkanukrauh, Pasuk; Nganvongpanit, Korakot

2016-01-01

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.

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

PubMed Central

Buddhachat, Kittisak; Klinhom, Sarisa; Siengdee, Puntita; Brown, Janine L.; Nomsiri, Raksiri; Kaewmong, Patcharaporn; Thitaram, Chatchote; Mahakkanukrauh, Pasuk; Nganvongpanit, Korakot

2016-01-01

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. PMID:27196603

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

NASA Astrophysics Data System (ADS)

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

2010-06-01

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

Digital Equivalent Data System for XRF Labeling of Objects

NASA Technical Reports Server (NTRS)

Schramm, Harry F.; Kaiser, Bruce

2005-01-01

A digital equivalent data system (DEDS) is a system for identifying objects by means of the x-ray fluorescence (XRF) spectra of labeling elements that are encased in or deposited on the objects. As such, a DEDS is a revolutionary new major subsystem of an XRF system. A DEDS embodies the means for converting the spectral data output of an XRF scanner to an ASCII alphanumeric or barcode label that can be used to identify (or verify the assumed or apparent identity of) an XRF-scanned object. A typical XRF spectrum of interest contains peaks at photon energies associated with specific elements on the Periodic Table (see figure). The height of each spectral peak above the local background spectral intensity is proportional to the relative abundance of the corresponding element. Alphanumeric values are assigned to the relative abundances of the elements. Hence, if an object contained labeling elements in suitably chosen proportions, an alphanumeric representation of the object could be extracted from its XRF spectrum. The mixture of labeling elements and for reading the XRF spectrum would be compatible with one of the labeling conventions now used for bar codes and binary matrix patterns (essentially, two-dimensional bar codes that resemble checkerboards). A further benefit of such compatibility is that it would enable the conversion of the XRF spectral output to a bar or matrix-coded label, if needed. In short, a process previously used only for material composition analysis has been reapplied to the world of identification. This new level of verification is now being used for "authentication."

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

NASA Astrophysics Data System (ADS)

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

2016-06-01

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

Preliminary Study to Test the Feasibility of Sex Identification of Human (Homo sapiens) Bones Based on Differences in Elemental Profiles Determined by Handheld X-ray Fluorescence.

PubMed

Nganvongpanit, Korakot; Buddhachat, Kittisak; Brown, Janine L; Klinhom, Sarisa; Pitakarnnop, Tanita; Mahakkanukrauh, Pasuk

2016-09-01

Sex assignment of human remains is a crucial step in forensic anthropological studies. The aim of this study was to examine elemental differences between male and female bones using X-ray fluorescence (XRF) and determine if elemental profiling could be used for sex discrimination. Cranium, humerus, and os coxae of 60 skeletons (30 male, 30 female) from the Chiang Mai University Skeletal Collection were scanned by XRF and differences in elemental profiles between male and female bones determined using discriminant analysis. In the cranium, three elements (S, Ca, Pb) were significantly higher in males and five elements (Si, Mn, Fe, Zn, Ag) plus light elements (atomic number lower than 12) were higher in females. In humerus and os coxae, nine elements were significantly higher in male and one element was higher in female samples. The accuracy rate for sex estimation was 60, 63, and 61 % for cranium, humerus, and os coxae, respectively, and 67 % when data for all three bones were combined. We conclude that there are sex differences in bone elemental profiles; however, the accuracy of XRF analyses for discriminating between male and female samples was low compared to standard morphometric and molecular methods. XRF could be used on small samples that cannot be sexed by traditional morphological methods, but more work is needed to increase the power of this technique for gender assignment.

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

PubMed

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

2012-02-01

X-ray imaging offers a new 3-D view into cells. With its ability to penetrate whole hydrated cells it is ideally suited for pairing fluorescence light microscopy and nanoscale X-ray tomography. In this paper, we describe the X-ray optical set-up and the design of the cryo full-field transmission X-ray microscope (TXM) at the electron storage ring BESSY II. Compared to previous TXM set-ups with zone plate condenser monochromator, the new X-ray optical layout employs an undulator source, a spherical grating monochromator and an elliptically shaped glass capillary mirror as condenser. This set-up improves the spectral resolution by an order of magnitude. Furthermore, the partially coherent object illumination improves the contrast transfer of the microscope compared to incoherent conditions. With the new TXM, cells grown on flat support grids can be tilted perpendicular to the optical axis without any geometrical restrictions by the previously required pinhole for the zone plate monochromator close to the sample plane. We also developed an incorporated fluorescence light microscope which permits to record fluorescence, bright field and DIC images of cryogenic cells inside the TXM. For TXM tomography, imaging with multi-keV X-rays is a straightforward approach to increase the depth of focus. Under these conditions phase contrast imaging is necessary. For soft X-rays with shrinking depth of focus towards 10nm spatial resolution, thin optical sections through a thick specimen might be obtained by deconvolution X-ray microscopy. As alternative 3-D X-ray imaging techniques, the confocal cryo-STXM and the dual beam cryo-FIB/STXM with photoelectron detection are proposed. Copyright © 2012 Elsevier Inc. All rights reserved.

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

PubMed

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

2016-09-01

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

Trace Element Mapping of a Biological Specimen by a Full-Field X-ray Fluorescence Imaging Microscope with a Wolter Mirror

NASA Astrophysics Data System (ADS)

Hoshino, Masato; Yamada, Norimitsu; Ishino, Toyoaki; Namiki, Takashi; Watanabe, Norio; Aoki, Sadao

2007-01-01

A full-field X-ray fluorescence imaging microscope with a Wolter mirror was applied to the element mapping of alfalfa seeds. The X-ray fluorescence microscope was built at the Photon Factory BL3C2 (KEK). X-ray fluorescence images of several growing stages of the alfalfa seeds were obtained. X-ray fluorescence energy spectra were measured with either a solid state detector or a CCD photon counting method. The element distributions of iron and zinc which were included in the seeds were obtained using a photon counting method.

Nanoscale quantification of intracellular element concentration by X-ray fluorescence microscopy combined with X-ray phase contrast nanotomography

NASA Astrophysics Data System (ADS)

Gramaccioni, Chiara; Yang, Yang; Procopio, Alessandra; Pacureanu, Alexandra; Bohic, Sylvain; Malucelli, Emil; Iotti, Stefano; Farruggia, Giovanna; Bukreeva, Inna; Notargiacomo, Andrea; Fratini, Michela; Valenti, Piera; Rosa, Luigi; Berlutti, Francesca; Cloetens, Peter; Lagomarsino, Stefano

2018-01-01

We present here a correlative X-ray microscopy approach for quantitative single cell imaging of molar concentrations. By combining the elemental content provided by X-ray fluorescence microscopy and the morphology information extracted from X-ray phase nanotomography, we determine the intracellular molarity distributions. This correlative method was demonstrated on a freeze-dried human phagocytic cell to obtain the absolute elemental concentration maps of K, P, and Fe. The cell morphology results showed a very good agreement with atomic-force microscopy measurements. This work opens the way for non-destructive single cell chemical analysis down to the sub-cellular level using exclusively synchrotron radiation techniques. It will be of high interest in the case where it is difficult to access the morphology using atomic-force microscopy, for example, on frozen-hydrated cells or tissues.

Gaseous detectors for energy dispersive X-ray fluorescence analysis

NASA Astrophysics Data System (ADS)

Veloso, J. F. C. A.; Silva, A. L. M.

2018-01-01

The energy resolution capability of gaseous detectors is being used in the last years to perform studies on the detection of characteristic X-ray lines emitted by elements when excited by external radiation sources. One of the most successful techniques is the Energy Dispersive X-ray Fluorescence (EDXRF) analysis. Recent developments in the new generation of micropatterned gaseous detectors (MPGDs), triggered the possibility not only of recording the photon energy, but also of providing position information, extending their application to EDXRF imaging. The relevant features and strategies to be applied in gaseous detectors in order to better fit the requirements for EDXRF imaging will be reviewed and discussed, and some application examples will be presented.

Sample preparation for total reflection X-ray fluorescence analysis using resist pattern technique

NASA Astrophysics Data System (ADS)

Tsuji, K.; Yomogita, N.; Konyuba, Y.

2018-06-01

A circular resist pattern layer with a diameter of 9 mm was prepared on a glass substrate (26 mm × 76 mm; 1.5 mm thick) for total reflection X-ray fluorescence (TXRF) analysis. The parallel cross pattern was designed with a wall thickness of 10 μm, an interval of 20 μm, and a height of 1.4 or 0.8 μm. This additional resist layer did not significantly increase background intensity on the XRF peaks in TXRF spectra. Dotted residue was obtained from a standard solution (10 μL) containing Ti, Cr, Ni, Pb, and Ga, each at a final concentration of 10 ppm, on a normal glass substrate with a silicone coating layer. The height of the residue was more than 100 μm, where self-absorption in the large residue affected TXRF quantification (intensity relative standard deviation (RSD): 12-20%). In contrast, from a droplet composed of a small volume of solution dropped and cast on the resist pattern structure, the obtained residue was not completely film but a film-like residue with a thickness less than 1 μm, where self-absorption was not a serious problem. In the end, this sample preparation was demonstrated to improve TXRF quantification (intensity RSD: 2-4%).

Fluorescence X-ray microscopy on hydrated tributyltin-clay mineral suspensions

NASA Astrophysics Data System (ADS)

Neuhäusler, U.; Schmidt, C.; Hoch, M.; Susini, J.

2003-03-01

Using the scanning transmission X-ray microscope at ID21 beamline of the ESRF in fluorescence mode, we mapped tin at a bulk concentration of 1000 μg(Sn)/ml within hydrated tributyltin (TBT)-clay mineral (Kaolinite) dispersion with sub-300 nm spatial resolution. Using the L absorption edges of tin at 3929, 4156 and 4465 eV fluorescence radiation was excited in tin atoms with incident photon energies of 4 and 4.5 keV. When using 4 keV radiation, only tin fluorescence is excited. For 4.5 keV X rays, both the fluorescence of tin and calcium (which is present in the solid phase) can be measured. Methodologically, we were interested in assessing and proving the possibilities and limitations of fluorescence mapping using the L absorption edges of tin, where the fluorescence yield is significantly lower compared to other elements with their K edges in the same energy range. Scientifically, organotin-clay mineral interactions are of environmental concern because this factor influences significantly the distribution of toxic TBT in the aquatic System. On one hand, the half-life of TBT deposited to the sediment phase increases, and consequently the time of its bioavailability. On the other hand, the adsorption process is reversible, which means that contaminated sediments can act as a source of pollution. The adsorption and desorption effects can be studied directly with high spatial resolution and brought into connection to the surface properties of the clay mineral under study as well as to other experimental parameters, like pH or salinity.

Spatial X-ray fluorescence micro-imaging of minerals in grain tissues of wheat and related genotypes.

PubMed

Singh, Sudhir P; Vogel-Mikuš, Katarina; Vavpetič, Primož; Jeromel, Luka; Pelicon, Primož; Kumar, Jitendra; Tuli, Rakesh

2014-08-01

Wheat and its related genotypes show distinct distribution patterns for mineral nutrients in maternal and filial tissues in grains. X-ray-based imaging techniques are very informative to identify genotypes with contrasting tissue-specific localization of different elements. This can help in the selection of suitable genotypes for nutritional improvement of food grain crops. Understanding mineral localization in cereal grains is important for their nutritional improvement. Spatial distribution of mineral nutrients (Mg, P, S, K, Ca, Fe, Zn, Mn and Cu) was investigated between and within the maternal and filial tissues in grains of two wheat cultivars (Triticum aestivum Cv. WH291 and WL711), a landrace (T. aestivum L. IITR26) and a related wild species Aegilops kotschyi, using micro-proton-induced X-ray emission (µ-PIXE) and micro-X-ray fluorescence (µ-XRF). Aleurone and scutellum were major storage tissues for macro (P, K, Ca and Mg) as well as micro (Fe, Zn, Cu and Mn) nutrients. Distinct elemental distribution patterns were observed in each of the four genotypes. A. kotschyi, the wild relative of wheat and the landrace, T. aestivum L. IITR26, accumulated more Zn and Fe in scutellum and aleurone than the cultivated wheat varieties, WH291 and WL711. The landrace IITR26, accumulated far more S in grains, Mn in scutellum, aleurone and embryo region, Ca and Cu in aleurone and scutellum, and Mg, K and P in scutellum than the other genotypes. Unlike wheat, lower Mn and higher Fe, Cu and Zn concentrations were noticed in the pigment strand of A. kotschyi. Multivariate statistical analysis, performed on mineral distribution in major grain tissues (aleurone, scutellum, endosperm and embryo region) resolved the four genotypes into distinct clusters.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Xin

1996-12-01

X-ray spectroscopy has long been used to elucidate electronic and structural information of molecules. One of the weaknesses of x-ray absorption is its sensitivity to all of the atoms of a particular element in a sample. Through out this thesis, a new technique for enhancing the site- and spin-selectivity of the x-ray absorption has been developed. By high resolution fluorescence detection, the chemical sensitivity of K emission spectra can be used to identify oxidation and spin states; it can also be used to facilitate site-selective X-ray Absorption Near Edge Structure (XANES) and site-selective Extended X-ray Absorption Fine Structure (EXAFS). Themore » 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.« less

JGIXA - A software package for the calculation and fitting of grazing incidence X-ray fluorescence and X-ray reflectivity data for the characterization of nanometer-layers and ultra-shallow-implants

NASA Astrophysics Data System (ADS)

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

2016-04-01

Grazing incidence XRF (GIXRF) is a very surface sensitive, nondestructive analytical tool making use of the phenomenon of total external reflection of X-rays on smooth polished surfaces. In recent years the method experienced a revival, being a powerful tool for process analysis and control in the fabrication of semiconductor based devices. Due to the downscaling of the process size for semiconductor devices, junction depths as well as layer thicknesses are reduced to a few nanometers, i.e. the length scale where GIXRF is highly sensitive. GIXRF measures the X-ray fluorescence induced by an X-ray beam incident under varying grazing angles and results in angle dependent intensity curves. These curves are correlated to the layer thickness, depth distribution and mass density of the elements in the sample. But the evaluation of these measurements is ambiguous with regard to the exact distribution function for the implants as well as for the thickness and density of nanometer-thin layers. In order to overcome this ambiguity, GIXRF can be combined with X-ray reflectometry (XRR). This is straightforward, as both techniques use similar measurement procedures and the same fundamental physical principles can be used for a combined data evaluation strategy. Such a combined analysis removes ambiguities in the determined physical properties of the studied sample and, being a correlative spectroscopic method, also significantly reduces experimental uncertainties of the individual techniques. In this paper we report our approach to a correlative data analysis, based on a concurrent calculation and fitting of simultaneously recorded GIXRF and XRR data. Based on this approach we developed JGIXA (Java Grazing Incidence X-ray Analysis), a multi-platform software package equipped with a user-friendly graphic user interface (GUI) and offering various optimization algorithms. Software and data evaluation approach were benchmarked by characterizing metal and metal oxide layers on

The feasibility of in vivo detection of lanthanum using a 241Am K x-ray fluorescence system.

PubMed

Nguyen, Joanna; Keldani, Zaid; Da Silva, Eric; Pejović-Milić, Ana; Gräfe, James L

2017-08-21

Lanthanum (La) is commonly used in phosphate binders in the form of lanthanum carbonate in patients with end-stage kidney disease undergoing hemodialysis treatments. With this administration, there is the potential for La storage in the body with bone being the main site of concern. However, the long-term effects of residual La in the body on bone health are not yet known. In this work, we investigate the feasibility of using a K x-ray fluorescence (K-XRF) spectroscopy system to measure bone La in vivo. A series of hydroxyapatite (HAp) bone mineral phantoms were created to represent human bone. A 1.09 GBq 241 Am source was used to excite the HAp phantoms doped with various known concentrations of La placed in a 90° geometry relative to the photon source and high-purity germanium (HPGe) detector. For a detector live time of 2000 s, the minimum detection limit was calculated to be 1.7 µg La g -1 Ca or 0.7 µg La g -1 HAp and is comparable to previously reported in vivo bone La concentrations. The technique developed in this study shows promising results and provides an alternative method to invasive biopsy sampling techniques to monitor the accumulation of bone La. To the best of our knowledge, this is the first reported work that seeks to non-invasively measure bone La via in vivo XRF.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Das, Gangadhar; Kane, S. R.; Khooha, Ajay

2015-05-15

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

Mathematical simulations of photon interactions using Monte Carlo analysis to evaluate the uncertainty associated with in vivo K X-ray fluorescence measurements of stable lead in bone

NASA Astrophysics Data System (ADS)

Lodwick, Camille J.

This research utilized Monte Carlo N-Particle version 4C (MCNP4C) to simulate K X-ray fluorescent (K XRF) measurements of stable lead in bone. Simulations were performed to investigate the effects that overlying tissue thickness, bone-calcium content, and shape of the calibration standard have on detector response in XRF measurements at the human tibia. Additional simulations of a knee phantom considered uncertainty associated with rotation about the patella during XRF measurements. Simulations tallied the distribution of energy deposited in a high-purity germanium detector originating from collimated 88 keV 109Cd photons in backscatter geometry. Benchmark measurements were performed on simple and anthropometric XRF calibration phantoms of the human leg and knee developed at the University of Cincinnati with materials proven to exhibit radiological characteristics equivalent to human tissue and bone. Initial benchmark comparisons revealed that MCNP4C limits coherent scatter of photons to six inverse angstroms of momentum transfer and a Modified MCNP4C was developed to circumvent the limitation. Subsequent benchmark measurements demonstrated that Modified MCNP4C adequately models photon interactions associated with in vivo K XRF of lead in bone. Further simulations of a simple leg geometry possessing tissue thicknesses from 0 to 10 mm revealed increasing overlying tissue thickness from 5 to 10 mm reduced predicted lead concentrations an average 1.15% per 1 mm increase in tissue thickness (p < 0.0001). An anthropometric leg phantom was mathematically defined in MCNP to more accurately reflect the human form. A simulated one percent increase in calcium content (by mass) of the anthropometric leg phantom's cortical bone demonstrated to significantly reduce the K XRF normalized ratio by 4.5% (p < 0.0001). Comparison of the simple and anthropometric calibration phantoms also suggested that cylindrical calibration standards can underestimate lead content of a human leg up

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

2015-01-01

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

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

DOE PAGES

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

2015-01-23

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

A Practical Guide for the Preparation of Specimens for X-ray Fluorescence and X-ray Diffraction Analysis (by V. E. Buhrke, R. Jenkins, and D. K. Smith)

NASA Astrophysics Data System (ADS)

Rudman, Reuben

1999-06-01

Wiley-VCH: New York, 1998. xxiv + 333 pp. ISBN 0-471-19458-1. $79.95. I would have subtitled this book "All You Ever Wanted To Know about ...Sample Preparation". Although its principal thrust is geared towards the analytical chemist in an X-ray diffraction (XRD) or X-ray fluorescence (XRF) service laboratory, this text will be of use primarily as a reference source in all milieus dealing with undergraduate research projects and advanced laboratory courses in physical and analytical chemistry. It contains dozens of suggestions for preparing randomly oriented small samples of nearly anything. For example, rocks and minerals, soft organics and hard ceramics, radioactive and liquid materials, metals and oils are all treated. As the availability of XRD and XRF equipment has increased, so has the use of these techniques in the teaching schedule. Many undergraduate laboratory and research projects utilizing these methods have been described in the literature and are found in laboratory textbooks. Very often, especially with the increasingly common use of automated computer-controlled instrumentation, sample preparation has become the key experimental technique required for successful data collection. However, it is not always easy to prepare the statistically random distribution of small particles (crystallites) that is required by these methods. A multitude of techniques have been developed over the past 70 years, but many of them have been handed down by word of mouth or are scattered throughout the literature. This book represents an attempt to systematically describe the theory and practice of sample preparation. This excellent guide to the intricacies of sample preparation begins with a description of statistical sampling methods and the principles of grinding techniques. After a discussion of XRF specimen preparation, which includes pressing pellets, fusion methods, crucible selection and handling very small samples, detailed descriptions for handling rocks

Improvement of graphite crystal analyzer for light elements on X-ray fluorescence holography measurement

NASA Astrophysics Data System (ADS)

Happo, Naohisa; Hada, Takuma; Kubota, Atsushi; Ebisu, Yoshihiro; Hosokawa, Shinya; Kimura, Koji; Tajiri, Hiroo; Matsushita, Tomohiro; Hayashi, Kouichi

2018-05-01

Using a graphite crystal analyzer, focused monochromatic fluorescent X-rays can be obtained on an X-ray fluorescence holography (XFH) measurement. To measure the holograms of elements lighter than Ti, we improved a cylindrical-type crystal analyzer and constructed a small C-shaped analyzer. Using the constructed C-shaped analyzer, a Ca Kα hologram of a fluorite single crystal was obtained, from which we reconstructed a clear atomic image. The XFH measurements for the K, Ca, and Sc elements become possible using the presently constructed analyzer.

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

PubMed

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

2015-05-01

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

Synchrotron-induced X-ray fluorescence from rat bone and lumber vertebra of different age groups

NASA Astrophysics Data System (ADS)

Rao, Donepudi V.; Swapna, Medasani; Cesareo, Roberto; Brunetti, Antonio; Akatsuka, Tako; Yuasa, Tetsuya; Takeda, Tohoru; Tromba, Giuliana; Gigante, Giovanni E.

2009-02-01

The fluorescence spectra from rat bones of different age groups (8, 56 and 78 weeks) and lumber vertebra were measured with 8, 10 and 12 keV synchrotron X-rays. We have utilized the new hard X-ray micro-spectroscopy beamline facility, X27A, available at NSLS with a primary beam spot size of the order of ˜10 μm. With this spatial resolution and high flux throughput, X-ray fluorescent intensities for Ca and other trace elements were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. Regarding the lumber vertebra, we acquired the fluorescence spectra from the left, right and middle portions and calcium accumulation was evaluated and compared with the other samples. We have identified the major trace elements of Ca, Ni, Fe and Zn and minor trace elements of Ti, Cr and Mn in the sample. The percentage of scattered radiation and trace element contributions from these samples were highlighted at different energies.

Probing Intracellular Element Concentration Changes during Neutrophil Extracellular Trap Formation Using Synchrotron Radiation Based X-Ray Fluorescence

PubMed Central

Niemiec, Maria J.; Laforce, Brecht; Garrevoet, Jan; Vergucht, Eva; De Rycke, Riet; Cloetens, Peter; Urban, Constantin F.; Vincze, Laszlo

2016-01-01

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. PMID:27812122

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

PubMed Central

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

2013-01-01

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

Astrobiological Significance of Definitive Mineralogical Analysis of Martian Surface Samples Using the CheMin XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Feldman, S. M.; Blake, D. F.; Sarrazin, P.; Bish, D. L.; Chipera, S. J.; Vaniman, D. T.; Collins, S.

2004-01-01

The search for evidence of habitability, or of extant or extinct life on Mars, will initially be a search for evidence of past or present conditions supportive of life. The three key requirements for the emergence of life are thought to be liquid water; a suitable energy source; and chemical building blocks. CheMin is a miniaturized XRD/XRF (X-Ray diffraction / X-ray fluorescence) instrument which has been developed for definitive mineralogic analysis of soils and rocks on the Martian surface. The CheMin instrument can provide information that is highly relevant to each of these habitability requirements as summarized below.

X-ray ptychographic and fluorescence microscopy of frozen-hydrated cells using continuous scanning

DOE PAGES

Deng, Junjing; Vine, David J.; Chen, Si; ...

2017-03-27

X-ray microscopy can be used to image whole, unsectioned cells in their native hydrated state. It complements the higher resolution of electron microscopy for submicrometer thick specimens, and the molecule-specific imaging capabilites of fluorescence light microscopy. We describe here the first use of fast, continuous x-ray scanning of frozen hydrated cells for simultaneous sub-20 nm resolution ptychographic transmission imaging with high contrast, and sub-100 nm resolution deconvolved x-ray fluorescence imaging of diffusible and bound ions at native concentrations, without the need to add specific labels. Here, by working with cells that have been rapidly frozen without the use of chemicalmore » fixatives, and imaging them under cryogenic conditions, we are able to obtain images with well preserved structural and chemical composition, and sufficient stability against radiation damage to allow for multiple images to be obtained with no observable change.« less

X-ray based extensometry

NASA Technical Reports Server (NTRS)

Jordan, E. H.; Pease, D. M.

1988-01-01

A totally new method of extensometry using an X-ray beam was proposed. The intent of the method is to provide a non-contacting technique that is immune to problems associated with density variations in gaseous environments that plague optical methods. X-rays are virtually unrefractable even by solids. The new method utilizes X-ray induced X-ray fluorescence or X-ray induced optical fluorescence of targets that have melting temperatures of over 3000 F. Many different variations of the basic approaches are possible. In the year completed, preliminary experiments were completed which strongly suggest that the method is feasible. The X-ray induced optical fluorescence method appears to be limited to temperatures below roughly 1600 F because of the overwhelming thermal optical radiation. The X-ray induced X-ray fluorescence scheme appears feasible up to very high temperatures. In this system there will be an unknown tradeoff between frequency response, cost, and accuracy. The exact tradeoff can only be estimated. It appears that for thermomechanical tests with cycle times on the order of minutes a very reasonable system may be feasible. The intended applications involve very high temperatures in both materials testing and monitoring component testing. Gas turbine engines, rocket engines, and hypersonic vehicles (NASP) all involve measurement needs that could partially be met by the proposed technology.

Electron and fluorescence spectra of a water molecule irradiated by an x-ray free-electron laser pulse

NASA Astrophysics Data System (ADS)

Schäfer, Julia M.; Inhester, Ludger; Son, Sang-Kil; Fink, Reinhold F.; Santra, Robin

2018-05-01

With the highly intense x-ray light generated by x-ray free-electron lasers (XFELs), molecular samples can be ionized many times in a single pulse. Here we report on a computational study of molecular spectroscopy at the high x-ray intensity provided by XFELs. Calculated photoelectron, Auger electron, and x-ray fluorescence spectra are presented for a single water molecule that reaches many electronic hole configurations through repeated ionization steps. The rich details shown in the spectra depend on the x-ray pulse parameters in a nonintuitive way. We discuss how the observed trends can be explained by the competition of microscopic electronic transition processes. A detailed comparison between spectra calculated within the independent-atom model and within the molecular-orbital framework highlights the chemical sensitivity of the spectral lines of multiple-hole configurations. Our results demonstrate how x-ray multiphoton ionization-related effects such as charge-rearrangement-enhanced x-ray ionization of molecules and frustrated absorption manifest themselves in the electron and fluorescence spectra.

In vivo evaluation of Fe in human skin employing X-Ray Fluorescence Methodology (XRF)

NASA Astrophysics Data System (ADS)

Estevam, M.; Appoloni, C. R.

2007-02-01

Recent technological improvements allow the method of in vivo XRF to provide useful sensibility for diagnostics or monitoring in biomedical applications. In cases of hereditary sanguine disorders as the β-thalassaemia or a genetic disorder like Haemochromatosis, there is a high concentration of elements as Fe, Zn and Cu in the skin and internal organs, due to the treatment of those abnormalities or due to the own dysfunction caused by the disease. The levels of Fe related to the patient bearers of the β-thalassaemia are determined, at the moment, measuring a protein in the sanguine current, called ferritin. The monitoring of the protein is ineffective in several situations, such as when the patient suffers any disturbance of health. Nowadays, the main forms of measuring the levels of those metals through hepatic storage are the biopsy of the liver, that is invasive and potentially dangerous, presenting a rate of mortality of 0.1%, and by means of magnetic susceptibilities that employs a quantum superconductor, which is highly expensive and there are only three main world centers with this equipment This work investigates the use of a Si PIN-diode detector and a 238Pu source (13 and 17keV; 13%; 95.2mCi; 86y) for the measurement of Fe skin levels compatible with those associated to the disease β-thalassaemia. XRF spectra were analyzed using a set of AXIL-WinQXAS programs elaborated and disseminated by the IAEA. The determination coefficient of the calibration model (sensitivity curve) was 0.97. Measurements on skin phantoms containing concentrations of Fe in the range from 10 to 150 parts per million (ppm), indicate that we are able to detect Fe at levels of the order of 15ppm, using monitoring periods of 50 seconds and skin entrance dose less than 10 mSv, The literature reports skin Fe levels from 15.0 to 60.0 ppm in normal persons and from 70 to 150 ppm in thalassaemics patients. So, the employed methodology allows the measurement of the skin Fe concentration.

2D-3D μXRF elemental mapping of archeological samples

NASA Astrophysics Data System (ADS)

Hampai, D.; Liedl, A.; Cappuccio, G.; Capitolo, E.; Iannarelli, M.; Massussi, M.; Tucci, S.; Sardella, R.; Sciancalepore, A.; Polese, C.; Dabagov, S. B.

2017-07-01

Recently opened for users at LNF XLab-Frascati a μ XRF station, named "Rainbow X-ray" - RXR, has been optimized for most of X-ray analytical research fields. The basic principle of the station is in the use of various geometrical combinations of polycapillary optics for X-ray beam shaping (focusing/collimation) at specially designed laboratory unit. In this work we have presented the results of archaeological studies on the artifacts of Paleolithic period and Iron Age (9th century BC to the midway of the 8th BC). The elemental analysis of these artifacts has been first performed by compact laboratory setup. Superficial (2D) and bulk (3D) micro-fluorescence mapping provides useful informations for the geologists in order to identify the possible artifacts provenience and origin. The results presented in this work are a part of wider anthropological/archeological investigations aimed at the understanding of social and economical relations of prehistorical communities.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Synchrotron radiation based STXM analysis and micro-XRF mapping of differential expression of extracellular thiol groups by Acidithiobacillus ferrooxidans grown on Fe(2+) and S(0).

PubMed

Xia, Jin-Lan; Liu, Hong-Chang; Nie, Zhen-Yuan; Peng, An-An; Zhen, Xiang-Jun; Yang, Yun; Zhang, Xiu-Li

2013-09-01

The differential expression of extracellular thiol groups by Acidithiobacillus ferrooxidans grown on substrates Fe(2+) and S(0) was investigated by using synchrotron radiation based scanning transmission X-ray microscopy (STXM) imaging and microbeam X-ray fluorescence (μ-XRF) mapping. The extracellular thiol groups (SH) were first alkylated by iodoacetic acid forming Protein-SCH2COOH and then the P-SCH2COOH was marked by calcium ions forming P-SCH2COOCa. The STXM imaging and μ-XRF mapping of SH were based on analysis of SCH2COO-bonded Ca(2+). The results indicated that the thiol group content of A. ferrooxidans grown on S(0) is 3.88 times to that on Fe(2+). Combined with selective labeling of SH by Ca(2+), the STXM imaging and μ-XRF mapping provided an in situ and rapid analysis of differential expression of extracellular thiol groups. © 2013.

Cesium Speciation in Dust from Municipal Solid Waste and Sewage Sludge Incineration by Synchrotron Radiation Micro-X-ray Analysis.

PubMed

Shiota, Kenji; Takaoka, Masaki; Fujimori, Takashi; Oshita, Kazuyuki; Terada, Yasuko

2015-11-17

The chemical behavior of Cs in waste incineration processes is important to consider when disposing of radionuclide-contaminated waste from the Fukushima Daiichi nuclear power plant accident in Japan. To determine the speciation of Cs, we attempted the direct speciation of trace amounts of stable Cs in the dust from municipal solid waste incineration (MSWI) and sewage sludge incineration (SSI) by micro-X-ray fluorescence (μ-XRF) and micro-X-ray absorption fine structure (μ-XAFS) at the SPring-8 facility. The μ-XRF results revealed that locally produced Cs was present in MSWI and SSI dust within the cluster size range of 2-10 μm. The μ-XAFS analysis confirmed that the speciation of Cs in MSWI dust was similar to that of CsCl, while in SSI dusts it was similar to pollucite. The solubility of Cs was considered to be influenced by the exact Cs species present in incineration residue.

Evaluation of a new optic-enabled portable X-ray fluorescence spectrometry instrument for measuring toxic metals/metalloids in consumer goods and cultural products

NASA Astrophysics Data System (ADS)

Guimarães, Diana; Praamsma, Meredith L.; Parsons, Patrick J.

2016-08-01

X-ray fluorescence spectrometry (XRF) is a rapid, non-destructive multi-elemental analytical technique used for determining elemental contents ranging from percent down to the μg/g level. Although detection limits are much higher for XRF compared to other laboratory-based methods, such as inductively coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectrometry (OES) and atomic absorption spectrometry (AAS), its portability and ease of use make it a valuable tool, especially for field-based studies. A growing necessity to monitor human exposure to toxic metals and metalloids in consumer goods, cultural products, foods and other sample types while performing the analysis in situ has led to several important developments in portable XRF technology. In this study, a new portable XRF analyzer based on the use of doubly curved crystal optics (HD Mobile®) was evaluated for detecting toxic elements in foods, medicines, cosmetics and spices used in many Asian communities. Two models of the HD Mobile® (a pre-production and a final production unit) were investigated. Performance parameters including accuracy, precision and detection limits were characterized in a laboratory setting using certified reference materials (CRMs) and standard solutions. Bias estimates for key elements of public health significance such as As, Cd, Hg and Pb ranged from - 10% to 11% for the pre-production, and - 14% to 16% for the final production model. Five archived public health samples including herbal medicine products, ethnic spices and cosmetic products were analyzed using both XRF instruments. There was good agreement between the pre-production and final production models for the four key elements, such that the data were judged to be fit-for-purpose for the majority of samples analyzed. Detection of the four key elements of interest using the HD Mobile® was confirmed using archived samples for which ICP-OES data were available based on digested sample materials. The HD

Simulating real-world field-based petrologic research in a field course: Incorporation of portable X-ray fluorescence spectrometry in the Iceland Volcanology Field Camp

NASA Astrophysics Data System (ADS)

Jordan, B.

2016-12-01

Field-based petrologic research projects often involve multiple field seasons, with geochemical analysis of samples collected in one season informing aspects of subsequent field seasons. To simulate this approach in the Iceland Volcanology Field Camp (South Dakota School of Mines & Technology) a portable X-ray fluorescence spectrometer (pXRF) was employed to provide "laboratory analyses" in support of a course mapping project. The project was conducted in the Árnes central volcano in the Neogene plateau lava succession in the West Fjords of northwestern Iceland. The field area has a wide compositional spectrum from basalt to rhyolite, with abundant intermediates. The pXRF is particularly helpful in the study of these kinds of rocks in Iceland because lithologies can be quite similar across a wide range of compositions (often lacking diagnostic macroscopic phenocryst assemblages, and having similar groundmass characteristics). A Bruker Tracer III-SD pXRF was utilized, operating at 40 KeV and 11.2 μA with no filter. Analyses were conducted at basecamp in the evenings on relatively flat fresh surfaces, with three 30 s analyses of different spots for each sample. A basic empirical calibration was generated with six aphyric samples previously analyzed by laboratory XRF. Light elements Na, Mg, and Al were not determined directly, but were estimated based on linear or polynomial correlations with other elements or elemental ratios (K, Ca, and Sr/Y respectively) determined from a previously obtained laboratory XRF data set for this central volcano. The resulting chemical analyses (normalized to sum to 100%) provided full major and minor element compositions to be used for classification, and several trace elements (V, Sr, Y, Zr) that could potentially distinguish different lavas of similar major element composition. The approach is coarse, and has pitfalls particularly regarding porphyritic rocks, but serves the objectives of the field camp project.

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

NASA Astrophysics Data System (ADS)

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

2017-03-01

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

Virtual bronchoscopic navigation without X-ray fluoroscopy to diagnose peripheral pulmonary lesions: a randomized trial.

PubMed

Asano, Fumihiro; Ishida, Takashi; Shinagawa, Naofumi; Sukoh, Noriaki; Anzai, Masaki; Kanazawa, Kenya; Tsuzuku, Akifumi; Morita, Satoshi

2017-12-11

Transbronchial biopsy for peripheral pulmonary lesions is generally performed under X-ray fluoroscopy. Virtual bronchoscopic navigation (VBN) is a method in which virtual images of the bronchial route to the lesion are produced based on CT images obtained before VBN, and the bronchoscope is guided using these virtual images, improving the diagnostic yield of peripheral pulmonary lesions. VBN has the possibility of eliminating the need for X-ray fluoroscopy in the bronchoscopic diagnosis of peripheral lesions. To determine whether VBN can be a substitute for X-ray fluoroscopy, a randomized multicenter trial (non-inferiority trial) was performed in VBN and X-ray fluoroscopy (XRF) -assisted groups. The non-inferiority margin in the VBN-assisted group compared with the XRF-assisted group was set at 15%. The subjects consisted of 140 patients with peripheral pulmonary lesions with a mean diameter > 3 cm. In the VBN-assisted group, the bronchoscope was guided to the lesion using a VBN system without X-ray fluoroscopy. In the XRF-assisted group, the same bronchoscope was guided to the lesion under X-ray fluoroscopy. Subsequently, in both groups, the lesion was visualized using endobronchial ultrasonography with a guide sheath (EBUS/GS), and biopsy was performed. In this serial procedure, X-ray fluoroscopy was not used in the VBNA group. The subjects of analysis consisted of 129 patients. The diagnostic yield was 76.9% (50/65) in the VBN-assisted group and 85.9% (55/64) in the XRF-assisted group. The difference in the diagnostic yield between the two groups was -9.0% (95% confidence interval: -22.3% ~ 4.3%). The non-inferiority of the VBN-assisted group could not be confirmed. The rate of visualizing lesions by EBUS was 95.4% (62/65) in the VBN-assisted group and 96.9% (62/64) in the XRF-assisted group, being high in both groups. On EBUS/GS, a bronchoscope and biopsy instruments may be guided to the lesions using VBN without X-ray fluoroscopy, but X-ray fluoroscopy is

Use of polarized radiation for increasing the sensitivity of multielement x-ray fluorescence analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ter-Saakov, A.A.; Glebov, M.V.

1985-10-01

An experimental x-ray fluorescence analysis facility has been developed using polarized radiation. A modernized small-sized REIS-I emitter is used as the x-ray genertor. Its characteristics are: a straight-through drift tube with a copper, molybdenum, or silver anode; and a controlled working voltage from 0 to 45 kV. The thickness of the inlet beryllium window is 100 um. Experiments were carried out on the facility on the optimization of fluorescence excitation conditions of biological samples. The investigations conducted of the dosimetric and spectral characteristics of the BS-1, BS-3, and BKh-7 x-ray tubes with copper, silver, and molybdenum anodes have shown thatmore » for the analysis in samples of biogenic elements, it is most efficient to use the BKh-7 and BS-1 tubes with a copper anode.« less

pXRF analyses of Louise Herreshoff's paintings in relation to CdS and other pigment degradation issues

NASA Astrophysics Data System (ADS)

Uffelman, Erich S.; Hobbs, Patricia A.; Barisas, Derek A. G.; Mass, Jennifer L.

2013-04-01

Portable X-ray Fluorescence Spectrometry (pXRF) was used to survey 33 works in Washington and Lee University's collection of Louise Herreshoff's paintings. This work was done both to support a condition assessment of the paintings and their pigments and to determine which paintings might be appropriate for further study in the context of ongoing key synchrotron research into the degradation mechanisms of cadmium sulfide yellow pigment (CdS).

The potential for portable X-ray fluorescence determination of soil copper at ancient metallurgy sites, and considerations beyond measurements of total concentrations.

PubMed

Tighe, M; Rogan, G; Wilson, S C; Grave, P; Kealhofer, L; Yukongdi, P

2018-01-15

Copper (Cu) at ancient metallurgy sites represents the earliest instance of anthropogenically generated metal pollution. Such sites are spread across a wide range of environments from Eurasia to South America, and provide a unique opportunity to investigate the past and present extent and impact of metalworking contamination. Establishing the concentration and extent of soil Cu at archaeometallurgy sites can enhance archaeological interpretations of site use but can also, more fundamentally, provide an initial indication of contamination risk from such sites. Systematic evaluations of total soil Cu concentrations at ancient metalworking sites have not been conducted, due in part to the limitations of conventional laboratory-based protocols. In this paper, we first review what is known about Cu soil concentrations at ancient metallurgy sites. We then assess the benefits and challenges of portable X-ray fluorescence spectrometry (pXRF) as an alternative, rapid technique for the assessment of background and contaminant levels of Cu in soils. We conclude that pXRF is an effective tool for identifying potential contamination. Finally, we provide an overview of some major considerations beyond total Cu concentrations, such as bioavailability assessments, that will need to be considered at such sites to move toward a complete assessment of environmental and human risk. Copyright © 2017 Elsevier Ltd. All rights reserved.

Combined use of infrared and hard X-ray microprobes for spectroscopy-based neuroanatomy

NASA Astrophysics Data System (ADS)

Surowka, A. D.; Ziomber, A.; Czyzycki, M.; Migliori, A.; Pieklo, L.; Kasper, K.; Szczerbowska-Boruchowska, M.

2018-05-01

Understanding the pathological triggers that affect the structural and physiological integrity of biochemical milieu of neurons is crucial to extend our knowledge on brain disorders, that are in many circumstances hardly treatable. Over recently, by using sophisticated hyperspectral micro-imaging modalities, it has been placed within our reach to get an insight into high fidelity histological details along with corresponding biochemical information in a label-free fashion, without using any additional chemical fixatives. However, in order to push forwards extensive application of these methods in the clinical arena, it is viable to make further iterations in novel data analysis protocols in order to boost their sensitivity. Therefore, in our study we proposed a new combined approach utilizing both benchtop Fourier transform infrared (FTIR) and synchrotron X-ray fluorescence (SR-XRF) micro-spectroscopies coupled with multivariate data clustering using the K-means algorithm for combined molecular and elemental micro-imaging, so that these complimentary analytical tools could be used for delineating between various brain structures based on their biochemical composition. By utilizing mid-IR transmission FTIR experiments, the biochemical composition in terms of lipids, proteins and phosphodiesters became accessible. In turn, the SR-XRF experiment was carried out at the advanced IAEA X-ray spectrometry station at Elettra Sincrotrone Trieste. By measuring in vacuum and by using the primary exciting X-ray beam, monochromatized to 10.5 keV, we took advantage of accessing the characteristic X-ray lines of a variety of elements ranging from carbon to zinc. Herein, we can report that the developed methodology has high specificity for label-free discriminating between lipid- and protein-rich brain tissue areas.

In vivo evaluation of Fe in human skin employing X-Ray Fluorescence Methodology (XRF)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Estevam, M.; Appoloni, C. R.

2007-02-12

Recent technological improvements allow the method of in vivo XRF to provide useful sensibility for diagnostics or monitoring in biomedical applications. In cases of hereditary sanguine disorders as the {beta}-thalassaemia or a genetic disorder like Haemochromatosis, there is a high concentration of elements as Fe, Zn and Cu in the skin and internal organs, due to the treatment of those abnormalities or due to the own dysfunction caused by the disease. The levels of Fe related to the patient bearers of the {beta}-thalassaemia are determined, at the moment, measuring a protein in the sanguine current, called ferritin. The monitoring ofmore » the protein is ineffective in several situations, such as when the patient suffers any disturbance of health. Nowadays, the main forms of measuring the levels of those metals through hepatic storage are the biopsy of the liver, that is invasive and potentially dangerous, presenting a rate of mortality of 0.1%, and by means of magnetic susceptibilities that employs a quantum superconductor, which is highly expensive and there are only three main world centers with this equipment This work investigates the use of a Si PIN-diode detector and a 238Pu source (13 and 17keV; 13%; 95.2mCi; 86y) for the measurement of Fe skin levels compatible with those associated to the disease {beta}-thalassaemia. XRF spectra were analyzed using a set of AXIL-WinQXAS programs elaborated and disseminated by the IAEA. The determination coefficient of the calibration model (sensitivity curve) was 0.97. Measurements on skin phantoms containing concentrations of Fe in the range from 10 to 150 parts per million (ppm), indicate that we are able to detect Fe at levels of the order of 15ppm, using monitoring periods of 50 seconds and skin entrance dose less than 10 mSv, The literature reports skin Fe levels from 15.0 to 60.0 ppm in normal persons and from 70 to 150 ppm in thalassaemics patients. So, the employed methodology allows the measurement of the skin

Delineating Heavy Metal Sources with Environmental Magnetism, X-Ray Fluorescence, and Geospatial Analysis: Baton Rouge, Louisiana

NASA Astrophysics Data System (ADS)

Taylor, Delmetria

The objective of this study is to detect the presence of anthropogenic magnetic particles by measuring the magnetic signature of soil samples in Baton Rouge, LA. Baton Rouge is currently ranked third among the Unites States' most polluted cities, so it is necessary to locate the sources of the problem and find solutions (U.S. Environmental Protection Agency [EPA], 2014). Magnetic susceptibility is a property that is easily, quickly, and inexpensively determined. It provides a highly-sensitive measurement of the compositional changes of minerals in soil. Magnetic susceptibility is influenced both anthropogenically and naturally by lithological and pedological heavy metal content. In this study, roughly 260 km2 (110 mi2) were sampled within the Baton Rouge, Louisiana area, and multiple environmental settings were covered. Geospatial and x-ray fluorescence analysis (XRF) were used to correlate magnetic susceptibility measurements and indicate increased anthropogenic activity near major industrial areas and interstates. Soil samples were analyzed, and isothermal remanent magnetization (IRM) acquisition curves indicate the presence of high- and low coercivity minerals, presumably magnetite and hematite. Enhanced susceptibility measurements do not appear to be dominated by lithology or soil in this particular area.

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

PubMed Central

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

2015-01-01

Abstract. 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 ±120  deg with respect to the excitation beam. We imaged a 28-mm-diameter water phantom with 4-mm-diameter Eppendorf tubes containing gold solutions with concentrations of 0.06 to 0.1% Au. While all Au vials were detectable in the SDD L-shell XFCT image, none of the vials were visible in the CdTe L-shell XFCT image. The detectability limit of the presented L-shell XFCT SDD imaging setup was 0.007% Au, a concentration observed in small animal studies. PMID:26839910

Morphological and chemical information in fresh and vitrified ovarian tissues revealed by X-ray Microscopy and Fluorescence: observational study

NASA Astrophysics Data System (ADS)

Pascolo, L.; Venturin, I.; Gianoncelli, A.; Salomé, M.; Altissimo, M.; Bedolla, D. E.; Giolo, E.; Martinelli, M.; Luppi, S.; Romano, F.; Zweyer, M.; Ricci, G.

2018-06-01

Many clinical circumstances impose the necessity of collection and prolonged storage of gametes and/or ovarian tissue in order to preserve the reproduction potential of subjects. This is particularly appropriate in the case of young women and pre-pubertal girls undergoing chemotherapeutic treatments. The success of later assisted fertilization will depend on the suitable cooling protocols minimizing cryo-damages and preserving their biological function. The freeze-thaw processes of cryopreservation may induce, in fact, morphological and structural damages of oocytes and tissue mainly due to the formation of intracellular ice and to the toxicity of cryoprotectant. The most used cryo-protocol is the slow freezing procedure, but recently many authors have proposed vitrification as an alternative, because of its simplicity. The damage extent and the quality of follicles after cryopreservation are usually evaluated morphologically by conventional histological procedures, light and electron microscopy. Our laboratory, to further improve the evaluation and to better investigate damages, is adopting a combination of Synchrotron soft X-ray Microscopy (at TwinMic – Elettra) and XRF at different incident energies (at TwinMic – Elettra and ID21 – ESRF). X-ray techniques were performed on histological sections at micro and sub-micron resolution. Phase contrast and absorption images revealed changes in the compactness of the tissues, as well as cellular abnormalities revealed at sub-micrometric resolution. The distributions of the elements detected at 7.3 and 1.5 keV were compared and particularly Cl resulted to be indicative of follicle integrity. The results demonstrate the utility and the potential of X-ray microscopy and fluorescence in this research field.

Recent results of synchrotron radiation induced total reflection X-ray fluorescence analysis at HASYLAB, beamline L

NASA Astrophysics Data System (ADS)

Streli, C.; Pepponi, G.; Wobrauschek, P.; Jokubonis, C.; Falkenberg, G.; Záray, G.; Broekaert, J.; Fittschen, U.; Peschel, B.

2006-11-01

At the Hamburger Synchrotronstrahlungslabor (HASYLAB), Beamline L, a vacuum chamber for synchrotron radiation-induced total reflection X-ray fluorescence analysis, is now available which can easily be installed using the adjustment components for microanalysis present at this beamline. The detector is now in the final version of a Vortex silicon drift detector with 50-mm 2 active area from Radiant Detector Technologies. With the Ni/C multilayer monochromator set to 17 keV extrapolated detection limits of 8 fg were obtained using the 50-mm 2 silicon drift detector with 1000 s live time on a sample containing 100 pg of Ni. Various applications are presented, especially of samples which are available in very small amounts: As synchrotron radiation-induced total reflection X-ray fluorescence analysis is much more sensitive than tube-excited total reflection X-ray fluorescence analysis, the sampling time of aerosol samples can be diminished, resulting in a more precise time resolution of atmospheric events. Aerosols, directly sampled on Si reflectors in an impactor were investigated. A further application was the determination of contamination elements in a slurry of high-purity Al 2O 3. No digestion is required; the sample is pipetted and dried before analysis. A comparison with laboratory total reflection X-ray fluorescence analysis showed the higher sensitivity of synchrotron radiation-induced total reflection X-ray fluorescence analysis, more contamination elements could be detected. Using the Si-111 crystal monochromator also available at beamline L, XANES measurements to determine the chemical state were performed. This is only possible with lower sensitivity as the flux transmitted by the crystal monochromator is about a factor of 100 lower than that transmitted by the multilayer monochromator. Preliminary results of X-ray absorption near-edge structure measurements for As in xylem sap from cucumber plants fed with As(III) and As(V) are reported. Detection limits

Atmospheric Electron-induced X-Ray Spectrometer (AEXS) Instrument Development

NASA Technical Reports Server (NTRS)

Urgiles, E.; Wilcox, J. Z.; Toda, R.; Crisp, J.; George, T.

2005-01-01

Introduction: This paper describes the progress in data acquisition and establishing the observational capability of the AEXS instrument. The AEXS is a miniature instrument[1-4] based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam which enables nondestructive evaluation of sample surfaces in planetary ambient atmospheres. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum of the AEXS source from the outside ambient atmosphere. Thus eliminating the need for a vacuum pumped sample chamber as is common in all laboratory SEM s. The transmitted electrons impinge on the sample exciting XRF spectra from the irradiated spot on in-situ or collected samples with sub-mm to cm-scale spatial resolution at Mars atmospheric pressure. The AEXS system (Fig 1) consists of a high-energy (>10keV) electron gun encapsulated by the isolation membrane, an XRF detection and analyzer system, and a high voltage power supply. The XRF data are analyzed to determine the elemental abundance for the irradiated spots. The approach to demonstrating a proof of concept of the AEXS has been through 1) demonstrating the viability of microfabricated membranes, 2) assembling AEXS setups with increasingly integrated functional components, and 3) simulating the AEXS observational capabilities. The development of the instrument is described in detail in the poster paper[4] at this conference. This paper focuses on describing the progress of the AEXS instrument to acquire XRF data and using commercially available software to analyze the data streams and determine the accuracy, precision and resolution of the analysis compared to the certified elemental abundance.

Progress on the Development of the Next Generation X-ray Beam Position Monitors at the Advanced Photon Source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, S.H.; Yang, B.X.; Decker, G.

Accurate and stable x-ray beam position monitors (XBPMs) are ke y elements in obtaining the desired user beam stability in the Advanced Photon Source (APS). The next generat ion XBPMs for high heat load front ends (HHL FEs) have been designed to meet these requirements by utilizing Cu K-edge x-ray fluorescence (XRF) from a pair of copper absorbers and have been installed at the front ends (FEs) of the APS. Com missioning data showed a significant performance improvement over the existing photoemission-based XBPMs. While a similar design concept can be applied for the canted undulator front ends, where two undulatormore » beams are separated by 1.0-mrad, the lower beam power (< 10 kW) per undulator allows us to explore lower-cost solutions based on Compton scat tering from the diamond blades placed edge-on to the x- ray beam. A prototype of the Compton scattering XBPM system was i nstalled at 24-ID-A in May 2015. In this report, the design and test results for XRF-based XBPM and Compton scattering based XBPM are presented. Ongoing research related to the development of the next generation XBPMs on thermal contac t resistance of a joint between two solid bodies is also discussed« less

Progress on the development of the next generation x-ray beam position monitors at the advanced photon source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, S. H., E-mail: shlee@aps.anl.gov; Yang, B. X., E-mail: bxyang@aps.anl.gov; Decker, G., E-mail: decker@aps.anl.gov

Accurate and stable x-ray beam position monitors (XBPMs) are key elements in obtaining the desired user beam stability in the Advanced Photon Source (APS). The next generation XBPMs for high heat load front ends (HHL FEs) have been designed to meet these requirements by utilizing Cu K-edge x-ray fluorescence (XRF) from a pair of copper absorbers and have been installed at the front ends (FEs) of the APS. Commissioning data showed a significant performance improvement over the existing photoemission-based XBPMs. While a similar design concept can be applied for the canted undulator front ends, where two undulator beams are separatedmore » by 1.0-mrad, the lower beam power (< 10 kW) per undulator allows us to explore lower-cost solutions based on Compton scattering from the diamond blades placed edge-on to the x-ray beam. A prototype of the Compton scattering XBPM system was installed at 24-ID-A in May 2015. In this report, the design and test results for XRF-based XBPM and Compton scattering based XBPM are presented. Ongoing research related to the development of the next generation XBPMs on thermal contact resistance of a joint between two solid bodies is also discussed.« less

Cyclostratigraphic analysis of the Middle to lower Upper Ordovician Postolonnec Formation in the Armorican Massif (France): integrating pXRF, gammay-ray and lithological data

NASA Astrophysics Data System (ADS)

Sinnesael, Matthias; Loi, Alfredo; Dabard, Marie-Pierre; Vandenbroucke, Thijs; Claeys, Philippe

2017-04-01

The Middle to lower Upper Ordovician sections of the Crozon Peninsula area (Postolonnec Formation, Armorican Massif, western France) show multi-order eustatic sea-level changes (Dabard et al., 2015). The sections are characterized by siliciclastic facies, which were deposited in tidal to storm-dominated shelf environments. Dabard et al. (2015) analysed the facies, their stacking patterns, and gamma-ray data and applied backstripping to identify subsidence and several orders of sea-level change. The main stratigraphic constraints are coming from (chitinozoan) biostratigraphy. The 3th to 5th orders changes are hypothesized to correspond to various frequencies related to astronomical forcing. This study investigates the potential added value of portable X-Ray Fluorescence (pXRF) and the application of spectral analyses. High-resolution (cm-scale) non-destructive pXRF and natural gamma-ray measurements were carried out on 14 m of section that was equally logged on a cm resolution. The pXRF measurements on the surface of the outcrops are compared with earlier results of wavelength dispersive XRF spectrometry and ICP-MS. The potassium records of the pXRF and gamma-ray logs are comparable and essentially reflect lithological variations (i.e., between mudstone and coarse sandstones). Other reliably measured elements also reflected lithological aspects such as clay-sandstone alternations (e.g. K, Rb, Ti), placer locations (Zr, Ce, Ti) and potentially clay mineralogy and condensation horizons (Ni, Zn, Co, Mn). Spectral analyses of the various proxies (lithology, natural gamma-ray and pXRF) are compared with each other. Both the new high-resolution data (14 m of section) as well as the published low-resolution data (which span almost 400 m of Darriwilian-Sandbian) were analyzed. The study reveals strong indications for the imprint of obliquity, precession and eccentricity. Obtaining age constraints, in addition to the existing biostratigraphical framework is a challenge in

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu Di; Li Yuhua; Wong, Molly D.

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

Comparison of soil pollution concentrations determined using AAS and portable XRF techniques.

PubMed

Radu, Tanja; Diamond, Dermot

2009-11-15

Past mining activities in the area of Silvermines, Ireland, have resulted in heavily polluted soils. The possibility of spreading pollution to the surrounding areas through dust blow-offs poses a potential threat for the local communities. Conventional environmental soil and dust analysis techniques are very slow and laborious and consequently there is a need for fast and accurate analytical methods, which can provide real-time in situ pollution mapping. Laboratory-based aqua regia acid digestion of the soil samples collected in the area followed by the atomic absorption spectrophotometry (AAS) analysis confirmed very high pollution, especially by Pb, As, Cu, and Zn. In parallel, samples were analyzed using portable X-ray fluorescence radioisotope and miniature tube powered (XRF) NITON instruments and their performance was compared. Overall, the portable XRF instrument gave excellent correlation with the laboratory-based reference AAS method.

Development of High-Speed Fluorescent X-Ray Micro-Computed Tomography

NASA Astrophysics Data System (ADS)

Takeda, T.; Tsuchiya, Y.; Kuroe, T.; Zeniya, T.; Wu, J.; Lwin, Thet-Thet; Yashiro, T.; Yuasa, T.; Hyodo, K.; Matsumura, K.; Dilmanian, F. A.; Itai, Y.; Akatsuka, T.

2004-05-01

A high-speed fluorescent x-ray CT (FXCT) system using monochromatic synchrotron x rays was developed to detect very low concentration of medium-Z elements for biomedical use. The system is equipped two types of high purity germanium detectors, and fast electronics and software. Preliminary images of a 10mm diameter plastic phantom containing channels field with iodine solutions of different concentrations showed a minimum detection level of 0.002 mg I/ml at an in-plane spatial resolution of 100μm. Furthermore, the acquisition time was reduced about 1/2 comparing to previous system. The results indicate that FXCT is a highly sensitive imaging modality capable of detecting very low concentration of iodine, and that the method has potential in biomedical applications.

Correlative organelle fluorescence microscopy and synchrotron X-ray chemical element imaging in single cells.

PubMed

Roudeau, Stéphane; Carmona, Asuncion; Perrin, Laura; Ortega, Richard

2014-11-01

X-ray chemical element imaging has the potential to enable fundamental breakthroughs in the understanding of biological systems because chemical element interactions with organelles can be studied at the sub-cellular level. What is the distribution of trace metals in cells? Do some elements accumulate within sub-cellular organelles? What are the chemical species of the elements in these organelles? These are some of the fundamental questions that can be addressed by use of X-ray chemical element imaging with synchrotron radiation beams. For precise location of the distribution of the elements, identification of cellular organelles is required; this can be achieved, after appropriate labelling, by use of fluorescence microscopy. As will be discussed, this approach imposes some limitations on sample preparation. For example, standard immunolabelling procedures strongly modify the distribution of the elements in cells as a result of the chemical fixation and permeabilization steps. Organelle location can, however, be performed, by use of a variety of specific fluorescent dyes or fluorescent proteins, on living cells before cryogenic fixation, enabling preservation of element distribution. This article reviews the methods used for fluorescent organelle labelling and X-ray chemical element imaging and speciation of single cells. Selected cases from our work and from other research groups are presented to illustrate the potential of the combination of the two techniques.

Sorption and Distribution of Copper in Unsaturated Pseudomonas putida CZ1 Biofilms as Determined by X-Ray Fluorescence Microscopy ▿

PubMed Central

Chen, Guangcun; Chen, Xincai; Yang, Yuanqiang; Hay, Anthony G.; Yu, Xiaohan; Chen, Yingxu

2011-01-01

The spatial and temporal distribution of metals in unsaturated Pseudomonas putida CZ1 biofilms was determined using synchrotron-based X-ray fluorescence microscopy (XRF). It was found that Fe, Mn, and Ca were mainly distributed near the air-biofilm interface of a biofilm grown on 40 mM citrate, while there were two Fe-, Mn-, and Ca-rich layers within a biofilm grown on 10 mM citrate. The sorption of copper by biofilm grown in medium containing 10 mM citrate was rapid, with copper being found throughout the biofilm after only 1 h of exposure. Copper initially colocalized with Fe and Mn element layers in the biofilm and then precipitated in a 40-μm-thick layer near the air-biofilm interface when exposed for 12 h. Cu K-edge X-ray absorption near edge structure (XANES) analysis revealed that Cu was primarily bound with citrate within the biofilm, and the precipitate formed in the biofilm exposed to copper for 12 h was most similar to copper phosphate. LIVE/DEAD staining revealed that cells at the biofilm-membrane interface were mostly alive even when the copper concentration reached 80.5 mg copper g−1 biomass. This suggests that the biofilm matrix provided significant protection for cells in this area. These results significantly improve our understanding of metal acquisition, transportation, and immobilization in unsaturated biofilm systems. PMID:21642411

Comparing the detection of iron-based pottery pigment on a carbon-coated sherd by SEM-EDS and by Micro-XRF-SEM.

PubMed

Pendleton, Michael W; Washburn, Dorothy K; Ellis, E Ann; Pendleton, Bonnie B

2014-03-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis.

Comparing the Detection of Iron-Based Pottery Pigment on a Carbon-Coated Sherd by SEM-EDS and by Micro-XRF-SEM

PubMed Central

Pendleton, Michael W.; Washburn, Dorothy K.; Ellis, E. Ann; Pendleton, Bonnie B.

2014-01-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis. PMID:24600333

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

DOEpatents

Wang, Ching L.

1983-01-01

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

X-ray fluorescence investigation of gilded and enamelled silver: The case study of four medieval processional crosses from central Italy

NASA Astrophysics Data System (ADS)

Ferretti, Marco; Polese, Claudia; Roldán García, Clodoaldo

2013-05-01

The presence of multilayered structures is common in such cultural artefacts as paintings, corroded metals, objects that underwent a whatever form of surface qualification. One of the most usual and complete ways to investigate such structures is observing a cross section, which requires sampling. There are however situations where at least part of the stratigraphic information can be derived non-destructively: the literature shows that X-ray fluorescence (XRF) has frequently been used, in recent years, for this purpose, with special regard to paintings and gilded metals. Aim of this paper is to further explore the suitability of XRF-based techniques to characterise multilayered structures. This is achieved by introducing improvements, with respect to previous works, in both equipment and data processing. The method, that has been developed for gilded and enamelled silver artefacts, relies on optimum excitation conditions provided for silver and on the relationship existing between the ratio AgKα/AgKβ of its fluorescence lines and the gilding thickness itself. The coating (gilding or enamel) thickness is derived by verifying the condition CKα,Ag = CKβ,Ag, where CKα,Ag and CKβ,Ag are the mass fractions of silver calculated on the lines AgKα and AgKβ, respectively. The calculations are carried out by PyMCA, a Fundamental Parameters code that implements the analysis of multilayered samples. As a case study we investigated in situ the four processional crosses of Borbona, Sant'Elpidio, Rosciolo and Forcella, made of a wood core with attached gilt and embossed silver sheets and enamelled silver plates. The analyses allowed to distinguish ancient restorations from original parts, to characterise the enamels and find their composition consistent with the dates of manufacturing and, as regards the cross of Rosciolo, to hypothesize the contribution of different "hands" in its manufacturing.

Feasibility Study of Compton Cameras for X-ray Fluorescence Computed Tomography with Humans

PubMed Central

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

2017-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1973-01-01

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

Using X-ray Fluorescence to Date Petroglyphs

NASA Astrophysics Data System (ADS)

McNeil, James

2009-10-01

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

Intracellular distribution and stability of a luminescent rhenium(I) tricarbonyl tetrazolato complex using epifluorescence microscopy in conjunction with X-ray fluorescence imaging

DOE PAGES

Wedding, Jason L.; Harris, Hugh H.; Bader, Christie A.; ...

2016-11-23

Optical fluorescence microscopy was used in conjunction with X-ray fluorescence microscopy to monitor the stability and intracellular distribution of the luminescent rhenium(I) complex fac-[Re(CO) 3(phen)L], where phen = 1,10-phenathroline and L = 5-(4-iodophenyl)tetrazolato, in 22Rv1 cells. The rhenium complex showed no signs of ancillary ligand dissociation, a conclusion based on data obtained via X-ray fluorescence imaging aligning iodine and rhenium distributions. A diffuse reticular localisation was detected for the complex, in the nuclear/perinuclear region of cells, by either optical or X-ray fluorescence techniques. Furthermore, X-ray fluorescence also showed that the Re-I complex disrupted the homeostasis of some biologically relevant elements,more » such as chlorine, potassium and zinc.« less

An interlaboratory comparison of bone lead measurements via K-shell X-ray fluorescence spectrometry: validation against inductively coupled plasma mass spectrometry

PubMed Central

Bellis, David J.; Todd, Andrew C.

2012-01-01

109Cd-based K-shell X-ray fluorescence spectrometry (hereafter, for brevity, XRF) is used, often in epidemiological studies, to perform non-invasive, in vivo measurements of lead in bone. We conducted the first interlaboratory study of XRF via the circulation of nine goat tibiæ in which the mean lead value ranged from 4.0 µg g−1 to 55.3 µg g−1 bone mineral. The test tibiæ were subsequently analyzed via nitric acid digestion followed by lead determination by inductively coupled plasma mass spectrometry (ICP-MS) – along with certified reference materials for bone lead – thus providing measurement traceability to SI units. Analysis of dried bone for lead via nitric acid digestion and ICP-MS yields mass fraction data in units of µg g−1 dry weight. The mean bone lead value based on ICP-MS analysis ranged from 1.8 µg g−1 to 35.8 µg g−1 dry weight. For comparison purposes, XRF-measured Pb values (µg g−1 bone mineral) were converted into the ICP-MS-measured units (µg g−1dry weight bone) by multiplying the former by the average ash fraction from the nine tibiæ. Eight of the XRF systems did not yield a significant bias for any of the nine tibiæ; one system was biased for one of the tibiæ; two systems were biased for two tibiæ; one system was biased for four tibiæ; two systems (813-1 and 804-2) were biased for five tibiæ and one system (801-1) was biased for six of the nine tibiæ. Average bias for the systems (under those particular operating conditions) that were biased for the majority of samples ranged from −2.6 µg g−1 (−15.7%) to 5.1 µg g−1 (30.7%) dry weight bone. All participants now have the ICP-MS data, allowing any corrective actions deemed necessary to be implemented. The ICP-MS data, however, indicated that the lead mass fraction varied considerably with the sampling location within the tibiæ, to the extent of exceeding XRF variability for the higher lead values. Material heterogeneity is an unavoidable reality of

Investigation of gunshot residue patterns using milli-XRF-techniques: first experiences in casework

NASA Astrophysics Data System (ADS)

Schumacher, Rüdiger; Barth, Martin; Neimke, Dieter; Niewöhner, Ludwig

2010-06-01

The investigation of gunshot residue (GSR) patterns for shooting range estimation is usually based on visualizing the lead, copper, or nitrocellulose distributions on targets like fabric or adhesive tape by chemographic color tests. The method usually provides good results but has its drawbacks when it comes to the examination of ammunition containing lead-free primers or bloody clothing. A milli-X-ray fluorescence (m-XRF) spectrometer with a large motorized stage can help to circumvent these problems allowing the acquisition of XRF mappings of relatively large areas (up to 20 x 20 cm) in millimeter resolution within reasonable time (2-10 hours) for almost all elements. First experiences in GSR casework at the Forensic Science Institute of the Bundeskriminalamt (BKA) have shown, that m-XRF is a useful supplementation for conventional methods in shooting ranges estimation, which helps if there are problems in transferring a GSR pattern to secondary targets (e.g. bloody or stained garments) or if there is no suitable color test available for the element of interest. The resulting elemental distributions are a good estimate for the shooting range and can be evaluated by calculating radial distributions or integrated count rates of irregular shaped regions like pieces of human skin which are too small to be investigated with a conventional WD-XRF spectrometer. Beside a mapping mode the milli-XRF offers also point and line scan modes which can also be utilized in gunshot crime investigations as a quick survey tool to identify bullet holes based on the elements present in the wipe ring.

X-ray fluorescence surface contaminant analyzer: A feasibility study

NASA Technical Reports Server (NTRS)

Eldridge, Hudson B.

1988-01-01

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

Intracellular distribution and stability of a luminescent rhenium(i) tricarbonyl tetrazolato complex using epifluorescence microscopy in conjunction with X-ray fluorescence imaging.

PubMed

Wedding, J L; Harris, H H; Bader, C A; Plush, S E; Mak, R; Massi, M; Brooks, D A; Lai, B; Vogt, S; Werrett, M V; Simpson, P V; Skelton, B W; Stagni, S

2017-04-19

Optical epifluorescence microscopy was used in conjunction with X-ray fluorescence imaging to monitor the stability and intracellular distribution of the luminescent rhenium(i) complex fac-[Re(CO) 3 (phen)L], where phen = 1,10-phenathroline and L = 5-(4-iodophenyl)tetrazolato, in 22Rv1 cells. The rhenium complex showed no signs of ancillary ligand dissociation, a conclusion based on data obtained via X-ray fluorescence imaging aligning iodine and rhenium distributions. A diffuse reticular localisation was detected for the complex in the nuclear/perinuclear region of cells, by either optical or X-ray fluorescence imaging techniques. X-ray fluorescence also showed that the rhenium complex disrupted the homeostasis of some biologically relevant elements, such as chlorine, potassium and zinc.

Effect of iron oxide reductive dissolution on the transformation and immobilization of arsenic in soils: New insights from X-ray photoelectron and X-ray absorption spectroscopy.