Correlation between Wavelength Dispersive X-ray Fluorescence (WDXRF) analysis of hardened concrete for chlorides vs. Atomic Absorption (AA) analysis in accordance with AASHTO T- 260; sampling and testing for chloride ion in concrete and concrete raw mater

DOT National Transportation Integrated Search

2014-04-01

A correlation between Wavelength Dispersive X-ray Fluorescence(WDXRF) analysis of Hardened : Concrete for Chlorides and Atomic Absorption (AA) analysis (current method AASHTO T-260, procedure B) has been : found and a new method of analysis has been ...

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

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

Methods of chemical and phase composition analysis of gallstones

NASA Astrophysics Data System (ADS)

Suvorova, E. I.; Pantushev, V. V.; Voloshin, A. E.

2017-11-01

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.

Taking into Account Interelement Interference in X-Ray Fluorescence Analysis of Thin Two-Layer Ti/V Systems

NASA Astrophysics Data System (ADS)

Mashin, N. I.; Razuvaev, A. G.; Cherniaeva, E. A.; Gafarova, L. M.; Ershov, A. V.

2018-03-01

We propose a new method for determining the thickness of layers in x-ray fluorescence analysis of two-layer Ti/V systems, using easily fabricated standardized film layers obtained by sputter deposition of titanium on a polymer film substrate. We have calculated correction factors taking into account the level of attenuation for the intensity of the primary emission from the x-ray tube and the analytical line for the element of the bottom layer in the top layer, and the enhancement of the fluorescence intensity for the top layer by the emission of atoms in the bottom layer.

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.

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

NASA Astrophysics Data System (ADS)

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

2016-02-01

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

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.

Cone Beam X-Ray Luminescence Tomography Imaging Based on KA-FEM Method for Small Animals.

PubMed

Chen, Dongmei; Meng, Fanzhen; Zhao, Fengjun; Xu, Cao

2016-01-01

Cone beam X-ray luminescence tomography can realize fast X-ray luminescence tomography imaging with relatively low scanning time compared with narrow beam X-ray luminescence tomography. However, cone beam X-ray luminescence tomography suffers from an ill-posed reconstruction problem. First, the feasibility of experiments with different penetration and multispectra in small animal has been tested using nanophosphor material. Then, the hybrid reconstruction algorithm with KA-FEM method has been applied in cone beam X-ray luminescence tomography for small animals to overcome the ill-posed reconstruction problem, whose advantage and property have been demonstrated in fluorescence tomography imaging. The in vivo mouse experiment proved the feasibility of the proposed method.

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.

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

NASA Astrophysics Data System (ADS)

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

2007-01-01

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

Thickness determination of thin solid films by angle-resolved X-ray fluorescence spectrometry using monochromatized synchrotron radiation

NASA Astrophysics Data System (ADS)

Schmitt, W.; Drotbohm, P.; Rothe, J.; Hormes, J.; Ottermann, C. R.; Bange, K.

1995-05-01

Thickness measurements by the method of angle-resolved, self-ratio X-ray fluorescence spectrometry (AR/SR/XFS) have been carried out on thin solid films using monochromatized synchrotron radiation at the Bonn storage ring ELSA. Synchrotron radiation was monochromatized by means of a double-crystal monochromator and fluorescence radiation was detected by a Si(Li) semiconductor detector. The results for sample systems consisting of Au on Si, Cr on SiO2 and TiO2 on alkali-free glass are very satisfactory and agree well with results obtained by other methods.

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

Cho, H; Ding, H; Ziemer, B

Purpose: To investigate the feasibility of energy calibration and energy response characterization of a photon counting detector using x-ray fluorescence. Methods: A comprehensive Monte Carlo simulation study was done to investigate the influence of various geometric components on the x-ray fluorescence measurement. Different materials, sizes, and detection angles were simulated using Geant4 Application for Tomographic Emission (GATE) Monte Carlo package. Simulations were conducted using 100 kVp tungsten-anode spectra with 2 mm Al filter for a single pixel cadmium telluride (CdTe) detector with 3 × 3 mm2 in detection area. The fluorescence material was placed 300 mm away from both themore » x-ray source and the detector. For angular dependence measurement, the distance was decreased to 30 mm to reduce the simulation time. Compound materials, containing silver, barium, gadolinium, hafnium, and gold in cylindrical shape, were simulated. The object size varied from 5 to 100 mm in diameter. The angular dependence of fluorescence and scatter were simulated from 20° to 170° with an incremental step of 10° to optimize the fluorescence to scatter ratio. Furthermore, the angular dependence was also experimentally measured using a spectrometer (X-123CdTe, Amptek Inc., MA) to validate the simulation results. Results: The detection angle between 120° to 160° resulted in more optimal x-ray fluorescence to scatter ratio. At a detection angle of 120°, the object size did not have a significant effect on the fluorescence to scatter ratio. The experimental results of fluorescence angular dependence are in good agreement with the simulation results. The Kα and Kβ peaks of five materials could be identified. Conclusion: The simulation results show that the x-ray fluorescence procedure has the potential to be used for detector energy calibration and detector response characteristics by using the optimal system geometry.« less

An alignment method for mammographic X-ray spectroscopy under clinical conditions.

PubMed

Miyajima, S; Imagawa, K; Matsumoto, M

2002-09-01

This paper describes an alignment method for mammographic X-ray spectroscopy under clinical conditions. A pinhole, a fluorescent screen, a laser device and the case for a detector are used for alignment of the focal spot, a collimator and a detector. The method determines the line between the focal spot and the point of interest in an X-ray field radiographically. The method allows alignment for both central axis and off-axis directions.

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

Bazalova, M; Ahmad, M; Fahrig, R

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

The X-ray Fluorescence Microscopy Beamline at the Australian Synchrotron

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

Paterson, D.; Jonge, M. D. de; Howard, D. L.

2011-09-09

A hard x-ray micro-nanoprobe has commenced operation at the Australian Synchrotron providing versatile x-ray fluorescence microscopy across an incident energy range from 4 to 25 keV. Two x-ray probes are used to collect {mu}-XRF and {mu}-XANES for elemental and chemical microanalysis: a Kirkpatrick-Baez mirror microprobe for micron resolution studies and a Fresnel zone plate nanoprobe capable of 60-nm resolution. Some unique aspects of the beamline design and operation are discussed. An advanced energy dispersive x-ray fluorescence detection scheme named Maia has been developed for the beamline, which enables ultrafast x-ray fluorescence microscopy.

Measuring partial fluorescence yield using filtered detectors.

PubMed

Boyko, T D; Green, R J; Moewes, A; Regier, T Z

2014-07-01

Typically, X-ray absorption near-edge structure measurements aim to probe the linear attenuation coefficient. These measurements are often carried out using partial fluorescence yield techniques that rely on detectors having photon energy discrimination improving the sensitivity and the signal-to-background ratio of the measured spectra. However, measuring the partial fluorescence yield in the soft X-ray regime with reasonable efficiency requires solid-state detectors, which have limitations due to the inherent dead-time while measuring. Alternatively, many of the available detectors that are not energy dispersive do not suffer from photon count rate limitations. A filter placed in front of one of these detectors will make the energy-dependent efficiency non-linear, thereby changing the responsivity of the detector. It is shown that using an array of filtered X-ray detectors is a viable method for measuring soft X-ray partial fluorescence yield spectra without dead-time. The feasibility of this technique is further demonstrated using α-Fe2O3 as an example and it is shown that this detector technology could vastly improve the photon collection efficiency at synchrotrons and that these detectors will allow experiments to be completed with a much lower photon flux reducing X-ray-induced damage.

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

NASA Astrophysics Data System (ADS)

Huang, Rong; Limburg, Karin; Rohtla, Mehis

2017-05-01

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

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

PubMed

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

1969-01-01

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

X-ray microlaminography with polycapillary optics

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

Dabrowski, K. M.; Dul, D. T.; Wrobel, A.

2013-06-03

We demonstrate layer-by-layer x-ray microimaging using polycapillary optics. The depth resolution is achieved without sample or source rotation and in a way similar to classical tomography or laminography. The method takes advantage from large angular apertures of polycapillary optics and from their specific microstructure, which is treated as a coded aperture. The imaging geometry is compatible with polychromatic x-ray sources and with scanning and confocal x-ray fluorescence setups.

Fluorescence background subtraction technique for hybrid fluorescence molecular tomography/x-ray computed tomography imaging of a mouse model of early stage lung cancer.

PubMed

Ale, Angelique; Ermolayev, Vladimir; Deliolanis, Nikolaos C; Ntziachristos, Vasilis

2013-05-01

The ability to visualize early stage lung cancer is important in the study of biomarkers and targeting agents that could lead to earlier diagnosis. The recent development of hybrid free-space 360-deg fluorescence molecular tomography (FMT) and x-ray computed tomography (XCT) imaging yields a superior optical imaging modality for three-dimensional small animal fluorescence imaging over stand-alone optical systems. Imaging accuracy was improved by using XCT information in the fluorescence reconstruction method. Despite this progress, the detection sensitivity of targeted fluorescence agents remains limited by nonspecific background accumulation of the fluorochrome employed, which complicates early detection of murine cancers. Therefore we examine whether x-ray CT information and bulk fluorescence detection can be combined to increase detection sensitivity. Correspondingly, we research the performance of a data-driven fluorescence background estimator employed for subtraction of background fluorescence from acquisition data. Using mice containing known fluorochromes ex vivo, we demonstrate the reduction of background signals from reconstructed images and sensitivity improvements. Finally, by applying the method to in vivo data from K-ras transgenic mice developing lung cancer, we find small tumors at an early stage compared with reconstructions performed using raw data. We conclude with the benefits of employing fluorescence subtraction in hybrid FMT-XCT for early detection studies.

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.

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

NASA Astrophysics Data System (ADS)

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

2008-12-01

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

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.

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.

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

PubMed

Liu, Pan; Deng, Xiaoyan; Tang, Xin; Shen, Shijian

2017-05-01

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

Method and apparatus for diagnosis of lead toxicity

DOEpatents

Rosen, John F.; Slatkin, Daniel N.; Wielopolski, Lucian

1989-01-01

Improved methods and apparatus for in vivo measurement of the skeletal lead burden of a patient and for diagnosis of lead toxicity are disclosed. The apparatus comprises an x-ray tube emitting soft low energy x-rays from a silver anode, a polarizer for polarizing the emitted x-rays, and a detector for detecting photons fluoresced from atoms in the patient's tibia upon irradiation by the polarized x-rays. The fluoresced photons are spectrally analyzed to determine their energy distribution. Peaks indicating the presence of lead are identified if the patient has relatively high bone lead content. The data may be compared to data recorded with respect to a similar test performed on patients having also had the conventional EDTA chelation tests performed thereon in order to correlate the test results with respect to a particular patient to the conventionally accepted EDTA chelation test.

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.

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

USGS Publications Warehouse

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

1969-01-01

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

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.

Differentiation of dental restorative materials combining energy-dispersive X-ray fluorescence spectroscopy and post-mortem CT.

PubMed

Merriam, Tim; Kaufmann, Rolf; Ebert, Lars; Figi, Renato; Erni, Rolf; Pauer, Robin; Sieberth, Till

2018-06-01

Today, post-mortem computed tomography (CT) is routinely used for forensic identification. Mobile energy-dispersive X-ray fluorescence (EDXRF) spectroscopy of a dentition is a method of identification that has the potential to be easier and cheaper than CT, although it cannot be used with every dentition. In challenging cases, combining both techniques could facilitate the process of identification and prove to be advantageous over chemical analyses. Nine dental restorative material brands were analyzed using EDXRF spectroscopy. Their differentiability was assessed by comparing each material's x-ray fluorescence spectrum and then comparing the spectra to previous research investigating differentiability in CT. To verify EDXRF's precision and accuracy, select dental specimens underwent comparative electron beam excited x-ray spectroscopy (EDS) scans, while the impact of the restorative surface area was studied by scanning a row of dental specimens with varying restorative surface areas (n = 10). EDXRF was able to differentiate all 36 possible pairs of dental filling materials; however, dual-energy CT was only able to differentiate 33 out of 36. The EDS scans showed correlating x-ray fluorescence peaks on the x-ray spectra compared to our EDXRF. In addition, the surface area showed no influence on the differentiability of the dental filling materials. EDXRF has the potential to facilitate corpse identification by differentiating and comparing restorative materials, providing more information compared to post-mortem CT alone. Despite not being able to explicitly identify a brand without a control sample or database, its fast and mobile use could accelerate daily routines or mass victim identification processes. To achieve this goal, further development of EDXRF scanners for this application and further studies evaluating the method within a specific routine need to be performed.

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

A new background subtraction method for energy dispersive X-ray fluorescence spectra using a cubic spline interpolation

NASA Astrophysics Data System (ADS)

Yi, Longtao; Liu, Zhiguo; Wang, Kai; Chen, Man; Peng, Shiqi; Zhao, Weigang; He, Jialin; Zhao, Guangcui

2015-03-01

A new method is presented to subtract the background from the energy dispersive X-ray fluorescence (EDXRF) spectrum using a cubic spline interpolation. To accurately obtain interpolation nodes, a smooth fitting and a set of discriminant formulations were adopted. From these interpolation nodes, the background is estimated by a calculated cubic spline function. The method has been tested on spectra measured from a coin and an oil painting using a confocal MXRF setup. In addition, the method has been tested on an existing sample spectrum. The result confirms that the method can properly subtract the background.

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.

X ray based displacement measurement for hostile environments

NASA Technical Reports Server (NTRS)

Canistraro, Howard A.; Jordon, Eric H.; Pease, Douglas M.; Fralick, Gustave C.

1992-01-01

A new method on noncontacting, high temperature extensometry based on the focus and scanning of x rays is currently under development and shows great promise of overcoming limitations associated with available techniques. The chief advantage is the ability to make undisturbed measurements through stratified or flowing gases, smoke, and flame. The system is based on the ability to focus and scan low energy, hard x rays such as those emanating from copper or molybdenum sources. The x rays are focused into a narrow and intense line image which can be scanned onto targets that fluoresce secondary x ray radiation. The final goal of the system is the ability to conduct macroscopic strain measurements in hostile environments by utilizing two or more fluorescing targets. Current work is limited to displacement measurement of a single target with a resolution of 1.25 micro-m and a target temperature of 1200 C, directly through an open flame. The main advantage of the technique lies in the penetrating nature of x rays which are not affected by the presence of refracting gas layers, smoke, flame, or intense thermal radiation, all of which could render conventional extensometry methods inoperative or greatly compromise their performance.

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 detector. The proposed x-ray fluorescence technique offers an accurate and efficient way to calibrate the energy response of a photon-counting detector. PMID:25471962

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

Determination of coal ash content by the combined x-ray fluorescence and scattering spectrum

NASA Astrophysics Data System (ADS)

Mikhailov, I. F.; Baturin, A. A.; Mikhailov, A. I.; Borisova, S. S.; Fomina, L. P.

2018-02-01

An alternative method is proposed for the determination of the inorganic constituent mass fraction (ash) in solid fuel by the ratio of Compton and Rayleigh X-ray scattering peaks IC/IR subject to the iron fluorescence intensity. An original X-ray optical scheme with a Ti/Mo (or Sc/Cu) double-layer secondary radiator allows registration of the combined fluorescence-and-scattering spectrum at the specified scattering angle. An algorithm for linear calibration of the Compton-to-Rayleigh IC/IR ratio is proposed which uses standard samples with two certified characteristics: mass fractions of ash (Ad) and iron oxide (WFe2O3). Ash mass fractions have been determined for coals of different deposits in the wide range of Ad from 9.4% to 52.7% mass and WFe2O3 from 0.3% to 4.95% mass. Due to the high penetrability of the probing radiation with energy E > 17 keV, the sample preparation procedure is rather simplified in comparison with the traditional method of Ad determination by the sum of fluorescence intensities of all constituent elements.

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.

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).

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.

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.

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.

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.

Philip A. Parilla | NREL

Science.gov Websites

atomic layer deposition for applications. He also manages the majority of X-ray characterization equipment at NREL, specifically X-ray diffraction and X-ray fluorescence instrumentation. Additionally, he for EERE's Hydrogen Storage program. He is also an expert in X-ray diffraction and X-ray fluorescence

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

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

A method of lead determination in human teeth by energy dispersive X-ray fluorescence (EDXRF).

PubMed

Sargentini-Maier, M L; Frank, R M; Leroy, M J; Turlot, J C

1988-12-01

A systematic sampling procedure was combined with a method of energy dispersive X-ray fluorescence (EDXRF) to study lead content and its variations in human teeth. On serial ground sections made on unembedded permanent teeth of inhabitants of Strasbourg with a special diamond rotating disk, 2 series of 500 microns large punch biopsies were made systematically in 5 directions from the tooth surface to the inner pulpal dentine with a micro-punching unit. In addition, pooled fragments of enamel and dentine were made for each tooth. On each punched fragment or pooled sample, lead content was determined after dissolution in ultrapure nitric acid, on a 4 microns thick polypropylene film, and irradiation with a Siemens EDXRF prototype with direct sample excitation by a high power X-ray tube with a molybdenum anode. Fluorescence was detected by a Si(Li) detector and calcium was used as an internal standard. This technique allowed a rapid, automatic, multielementary and non-destructive analysis of microsamples with good detection limits.

The use of wavelength dispersive X-ray fluorescence in the identification of the elemental composition of vanilla samples and the determination of the geographic origin by discriminant function analysis.

PubMed

Hondrogiannis, Ellen; Rotta, Kathryn; Zapf, Charles M

2013-03-01

Sixteen elements found in 37 vanilla samples from Madagascar, Uganda, India, Indonesia (all Vanilla planifolia species), and Papa New Guinea (Vanilla tahitensis species) were measured by wavelength dispersive X-ray fluorescence (WDXRF) spectroscopy for the purpose of determining the elemental concentrations to discriminate among the origins. Pellets were prepared of the samples and elemental concentrations were calculated based on calibration curves created using 4 Natl. Inst. of Standards and Technology (NIST) standards. Discriminant analysis was used to successfully classify the vanilla samples by their species and their geographical region. Our method allows for higher throughput in the rapid screening of vanilla samples in less time than analytical methods currently available. Wavelength dispersive X-ray fluorescence spectroscopy and discriminant function analysis were used to classify vanilla from different origins resulting in a model that could potentially serve to rapidly validate these samples before purchasing from a producer. © 2013 Institute of Food Technologists®

Migration of iron and manganese into CCA-treated wood in soil contact and the resulting error in leaching results when using energy dispersive x-ray fluorescence spectrometers

Treesearch

Tor P. Schultz; Darrel D. Nicholas; Stan Lebow

2003-01-01

In a laboratory leaching study, we found that chromated copper arsenate (CCA) treated wood, which had been exposed to one of five soils examined, unexpectedly appeared to gain significant Cr (47%) when measured with an energy-dispersive x-ray fluorescence instrument (American Wood-Preservers' Association (AWPA) Method A9-01 2001). Analysis of some of the leached...

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

The Intensity Modulation of the Fluorescent Line by a Finite Light Speed Effect in Accretion-powered X-Ray Pulsars

NASA Astrophysics Data System (ADS)

Yoshida, Yuki; Kitamoto, Shunji; Hoshino, Akio

2017-11-01

The X-ray line diagnostic method is a powerful tool for an investigation of plasma around accretion-powered X-ray pulsars. We point out an apparent intensity modulation of emission lines, with their rotation period of neutron stars, due to the finite speed of light (we call this effect the “finite light speed effect”) if the line emission mechanism is a kind of reprocessing, such as fluorescence or recombination after ionization by X-ray irradiation from pulsars. The modulation amplitude is determined by the size of the emission region, which is in competition with the smearing effect by the light crossing time in the emission region. This is efficient if the size of the emission region is roughly comparable to that of the rotation period multiplied by the speed of light. We apply this effect to a symbiotic X-ray pulsar, GX 1+4, where a spin modulation of the intense iron line of which has been reported. The finite light speed effect can explain the observed intensity modulation if its fluorescent region is the size of ˜ {10}12 cm.

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.

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

PubMed Central

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

2014-01-01

Purpose: To develop an accurate and comprehensive Monte Carlo (MC) model of an experimental benchtop polychromatic cone-beam x-ray fluorescence computed tomography (XFCT) setup and apply this MC model to optimize incident x-ray spectrum for improving production/detection of x-ray fluorescence photons from gold nanoparticles (GNPs). Methods: A detailed MC model, based on an experimental XFCT system, was created using the Monte Carlo N-Particle (MCNP) transport code. The model was validated by comparing MC results including x-ray fluorescence (XRF) and scatter photon spectra with measured data obtained under identical conditions using 105 kVp cone-beam x-rays filtered by either 1 mm of lead (Pb) or 0.9 mm of tin (Sn). After validation, the model was used to investigate the effects of additional filtration of the incident beam with Pb and Sn. Supplementary incident x-ray spectra, representing heavier filtration (Pb: 2 and 3 mm; Sn: 1, 2, and 3 mm) were computationally generated and used with the model to obtain XRF/scatter spectra. Quasimonochromatic incident x-ray spectra (81, 85, 90, 95, and 100 keV with 10 keV full width at half maximum) were also investigated to determine the ideal energy for distinguishing gold XRF signal from the scatter background. Fluorescence signal-to-dose ratio (FSDR) and fluorescence-normalized scan time (FNST) were used as metrics to assess results. Results: Calculated XRF/scatter spectra for 1-mm Pb and 0.9-mm Sn filters matched (r ≥ 0.996) experimental measurements. Calculated spectra representing additional filtration for both filter materials showed that the spectral hardening improved the FSDR at the expense of requiring a much longer FNST. In general, using Sn instead of Pb, at a given filter thickness, allowed an increase of up to 20% in FSDR, more prominent gold XRF peaks, and up to an order of magnitude decrease in FNST. Simulations using quasimonochromatic spectra suggested that increasing source x-ray energy, in the investigated range of 81–100 keV, increased the FSDR up to a factor of 20, compared to 1 mm Pb, and further facilitated separation of gold XRF peaks from the scatter background. Conclusions: A detailed MC model of an experimental benchtop XFCT system has been developed and validated. In exemplary calculations to illustrate the usefulness of this model, it was shown that potential use of quasimonochromatic spectra or judicious choice of filter material/thickness to tailor the spectrum of a polychromatic x-ray source can significantly improve the performance of benchtop XFCT, while considering trade-offs between FSDR and FNST. As demonstrated, the current MC model is a reliable and powerful computational tool that can greatly expedite the further development of a benchtop XFCT system for routine preclinical molecular imaging with GNPs and other metal probes. PMID:25281958

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

Ding, Huanjun; Cho, Hyo-Min; Molloi, Sabee, E-mail: symolloi@uci.edu

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 diametermore » 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 detector. The proposed x-ray fluorescence technique offers an accurate and efficient way to calibrate the energy response of a photon-counting detector.« less

Direct method for imaging elemental distribution profiles with long-period x-ray standing waves

NASA Astrophysics Data System (ADS)

Kohli, Vaibhav; Bedzyk, Michael J.; Fenter, Paul

2010-02-01

A model-independent Fourier-inversion method for imaging elemental profiles from multilayer and total-external reflection x-ray standing wave (XSW) data is developed for the purpose of understanding the assembly of atoms, ions, and molecules at well-defined interfaces in complex environments. The direct-method formalism is derived for the case of a long-period XSW generated by low-angle specular reflection in an attenuating overlayer medium. It is validated through comparison with simulated and experimental data to directly obtain an elemental distribution contained within the overlayer. We demonstrate this formalism by extracting the one-dimensional profile of Ti normal to the surface for a TiO2/Si/Mo trilayer deposited on a Si substrate using the TiKα fluorescence yield measured in air and under an aqueous electrolyte. The model-independent results demonstrate reduced coherent fractions for the in situ results associated with an incoherency of the x-ray beam (which are attributed to fluorescence excitation by diffusely or incoherently scattered x-rays). The uniqueness and limitations of the approach are discussed.

Calculation of K-shell fluorescence yields for low-Z elements

NASA Astrophysics Data System (ADS)

Nekkab, M.; Kahoul, A.; Deghfel, B.; Aylikci, N. Küp; Aylikçi, V.

2015-03-01

The analytical methods based on X-ray fluorescence are advantageous for practical applications in a variety of fields including atomic physics, X-ray fluorescence surface chemical analysis and medical research and so the accurate fluorescence yields (ωK) are required for these applications. In this contribution we report a new parameters for calculation of K-shell fluorescence yields (ωK) of elements in the range of 11≤Z≤30. The experimental data are interpolated by using the famous analytical function (ωk/(1 -ωk)) 1 /q (were q=3, 3.5 and 4) vs Z to deduce the empirical K-shell fluorescence yields. A comparison is made between the results of the procedures followed here and those theoretical and other semi-empirical fluorescence yield values. Reasonable agreement was typically obtained between our result and other works.

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.

Simultaneous determination of thorium, niobium, lead, and zinc by photon-induced x-ray fluorescence of lateritic material

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

LaBrecque, J.J.; Adames, D.; Parker, W.C.

1981-01-01

A rapid method is presented for the simultaneous determinations of thorium, niobium, lead, and zinc in lateritic material from Cerro Impacto, Estado Bolivar, Venezuela. This technique uses a PDP - 11/05 processor - based photon induced x-ray fluorescence system. The total variations of approximately 5% for concentrations of approximately 1 and 10% for concentrations of approximately 0.1% were obtained with only 500 s of fluorescent time. The values obtained by this method were in agreement with values measured by conventional flame atomic absorption spectroscopy for lead and zinc. The values for thorium measured were in agreement with the reported valuesmore » for the reference materials supplied by NBL.« less

Methods for identification and verification using vacuum XRF system

NASA Technical Reports Server (NTRS)

Kaiser, Bruce (Inventor); Schramm, Fred (Inventor)

2005-01-01

Apparatus and methods in which one or more elemental taggants that are intrinsically located in an object are detected by x-ray fluorescence analysis under vacuum conditions to identify or verify the object's elemental content for elements with lower atomic numbers. By using x-ray fluorescence analysis, the apparatus and methods of the invention are simple and easy to use, as well as provide detection by a non line-of-sight method to establish the origin of objects, as well as their point of manufacture, authenticity, verification, security, and the presence of impurities. The invention is extremely advantageous because it provides the capability to measure lower atomic number elements in the field with a portable instrument.

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.

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.

The Determination of Metals in Welding Fume by X-RaySpectrometry

NASA Astrophysics Data System (ADS)

Kuznetsova, O. V.; Begunova, L. A.; Romanenko, S. V.; Solodsky, S. A.

2018-01-01

Analysis of the current hygienic situation in the welding production showed that the intensification of welding processes involves the deterioration of air quality, which negatively affects the welders health. Respiratory effects seen in full-time welders have included bronchitis, airway irritation, lung function changes, and a possible increase in the incidence of lung cancer. The metal concentration in the air of the working area have been determined using the photometric method of analysis, which involves the stage of decomposition of the sample material before analysis. However, losses of the analyzed elements are possible when the sample is decomposed. The X-ray fluorescence method of analysis has the advantage of being nondestructive. The investigations shown the data of photometric determination of metals in welding aerosols is 1.5÷2 times lower than the results of X-ray fluorescence analysis.

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

NASA Technical Reports Server (NTRS)

Ross, H. Richard

1993-01-01

A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

Analysis of elemental concentration censored distributions in breast malignant and breast benign neoplasm tissues

NASA Astrophysics Data System (ADS)

Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J.; Góźdź, S.; Majewska, U.; Pajek, M.

2007-07-01

The total reflection X-ray fluorescence method was applied to study the trace element concentrations in human breast malignant and breast benign neoplasm tissues taken from the women who were patients of Holycross Cancer Centre in Kielce (Poland). These investigations were mainly focused on the development of new possibilities of cancer diagnosis and therapy monitoring. This systematic comparative study was based on relatively large (˜ 100) population studied, namely 26 samples of breast malignant and 68 samples of breast benign neoplasm tissues. The concentrations, being in the range from a few ppb to 0.1%, were determined for thirteen elements (from P to Pb). The results were carefully analysed to investigate the concentration distribution of trace elements in the studied samples. The measurements of concentration of trace elements by total reflection X-ray fluorescence were limited, however, by the detection limit of the method. It was observed that for more than 50% of elements determined, the concentrations were not measured in all samples. These incomplete measurements were treated within the statistical concept called left-random censoring and for the estimation of the mean value and median of censored concentration distributions, the Kaplan-Meier estimator was used. For comparison of concentrations in two populations, the log-rank test was applied, which allows to compare the censored total reflection X-ray fluorescence data. Found statistically significant differences are discussed in more details. It is noted that described data analysis procedures should be the standard tool to analyze the censored concentrations of trace elements analysed by X-ray fluorescence methods.

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

Ding, H; Cho, H; Molloi, S

Purpose: To investigate the feasibility of energy response calibration of a Si strip photon-counting detector by using the x-ray fluorescence technique. Methods: X-ray fluorescence was generated by using a pencil beam from a tungsten anode x-ray tube with 2 mm Al filtration. Spectra were acquired at 90° from the primary beam direction with an energy-resolved photon-counting detector based on Si strips. The distances from the source to target and the target to detector were approximately 19 and 11 cm, respectively. Four different materials, containing Ag, I, Ba, and Gd, were placed in small plastic aliquots with a diameter of approximatelymore » 0.7 cm for x-ray fluorescence measurements. Linear regression analysis was performed to derive the gain and offset values for the correlation between the measured fluorescence peak center and the known energies for materials. The energy resolution was derived from the full width at half maximum (FWHM) of the fluorescence peaks. In addition, the angular dependence of the recorded fluorescence spectra was studied at 30°, 60°, and 120°. Results: Strong fluorescence signals of all four target materials were recorded with the investigated geometry for the Si strip detector. The recorded pulse height was calibrated with respect to photon energy and the gain and offset values were calculated to be 7.0 mV/keV and −69.3 mV, respectively. Negligible variation in energy calibration was observed among the four energy thresholds. The variation among different pixels was estimated to be approximately 1 keV. The energy resolution of the detector was estimated to be 7.9% within the investigated energy range. Conclusion: The performance of a spectral imaging system using energy-resolved photon-counting detectors is very dependent on the energy calibration of the detector. The proposed x-ray fluorescence technique provides an accurate and efficient way to calibrate the energy response of a photon-counting detector.« less

Assessment of Ca and P content variation in enamel during an eight-week bleaching protocol using energy dispersive X-ray fluorescence

NASA Astrophysics Data System (ADS)

Sorozini, M.; Dos Santos, R. S.; Silva, E. M.; Dos Anjos, M. J.; Perez, C. R.

2017-05-01

Tooth bleaching is a simple technique performed with gels based on hydrogen peroxide molecules responsible for removing the tooth structure's pigmentation. The effects of the overuse of these agents on the tooth structure are not well established. Energy dispersive X-ray fluorescence (EDXRF) can be employed to analyze objects of biological origin as bone and tooth. It is very suitable analytical technique to detect demineralization processes in these tissues. The objective of this study was to use x-ray fluorescence to evaluate the effects on mineral content of enamel submitted to eight-week protocols of home bleaching gels (10% carbamide peroxide and 9.5% hydrogen peroxide), as well as bleaching strips. Four enamel fragments obtained from five teeth were subjected to bleaching for 8 weeks: Group 1- artificial saliva; Group 2-10% carbamide peroxide gel, 6 h daily; Group 3-9.5% hydrogen peroxide gel, two 30-minute applications; and Group 4-bleaching strips, twice daily for 30 min. The change in mineral content was assessed weekly using X-ray fluorescence (Artax 200). Differences were basically found in Group 4 for the concentrations of Ca and P after treatment with bleaching strips containing 10% hydrogen peroxide. For the Ca/P ratio, the differences were found in Group 2-15% carbamide peroxide (p < 0.05). X-ray fluorescence proved to be a suitable method for the evaluation of the mineral content, presenting the advantage of being able to evaluate the same area at different stages of the methodology.

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

Nekkab, M., E-mail: mohammed-nekkab@yahoo.com; LESIMS laboratory, Physics Department, Faculty of Sciences, University of Setif 1, 19000 Setif; Kahoul, A.

The analytical methods based on X-ray fluorescence are advantageous for practical applications in a variety of fields including atomic physics, X-ray fluorescence surface chemical analysis and medical research and so the accurate fluorescence yields (ω{sub K}) are required for these applications. In this contribution we report a new parameters for calculation of K-shell fluorescence yields (ω{sub K}) of elements in the range of 11≤Z≤30. The experimental data are interpolated by using the famous analytical function (ω{sub k}/(1−ω{sub k})){sup 1/q} (were q=3, 3.5 and 4) vs Z to deduce the empirical K-shell fluorescence yields. A comparison is made between the resultsmore » of the procedures followed here and those theoretical and other semi-empirical fluorescence yield values. Reasonable agreement was typically obtained between our result and other works.« less

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

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

Wedding, Jason L.; Harris, Hugh H.; Bader, Christie A.

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

Hard X-ray Ptychography: Making It Cool, Colorful and Fast

NASA Astrophysics Data System (ADS)

Deng, Junjing

Ptychography is a recently developed coherent imaging technique for extended objects, with a resolution not limited by the lens. Because X-rays have short wavelengths and high penetration ability, X-ray ptychography provides a powerful and unique tool for studying thick samples at high spatial resolution. We have advanced X-ray ptychography by making it cool, colorful, and fast. We make it cool by carrying out ptychography experiments at cryogenic conditions to image frozen-hydrated specimens. This largely removes the limitations of radiation damage on the achievable resolution, and allows one to obtain excellent preservation of structure and chemistry in biological specimens. We make it colorful by combining it with X-ray fluorescence measurements of chemical element distributions. In studies of biological specimens, this means that ptychography can reveal cellular ultrastructure at high contrast and at a resolution well beyond that of X-ray focusing optics, while X-ray fluorescence is used to simultaneously image the distribution of trace elements in cells (such as metals that play key roles in cell functions and which can be used in various disease therapeutic agents). Because X-ray fluorescence is not very sensitive for showing the light elements that comprise the majority of cellular materials, this combined approach provides the unique tool to obtain simultaneous views of ultrastructure and elemental compositions of specimens. We make it fast by using continuous-scan (or "fly-scan") methods. Conventional ptychography is implemented in a move-settle-measure approach, which is slow due to the positioning overheads. To overcome this bottleneck, we have developed fly-scan ptychography that is able to speed up the data collection, and real time on-site data analysis can be achieved by using a parallelized reconstruction code. With these advances, we conducted combined cryo X-ray ptychography and fluorescence imaging at 5.2 keV in a more practical way using fly scan, well-preserved cryogenic samples and rapid reconstructions, and obtained images of a whole frozen-hydrated eukaryotic cell at 18 nm resolution which we believe to be the highest spatial resolution obtained in X-ray imaging of frozen-hydrated biological samples to date. After a successful demonstration of fly-scan 3D ptychography on a gold test sample, we also obtained fly-scan 3D ptychography and fluorescence data on frozen-hydrated cells with an imaging speedup of factor more than 7. Finally, we applied fly-scan X-ray ptychography on un-thinned integrated circuits (ICs) using 10 keV X-rays, and were able to see the circuit details within the thick IC chips with a high resolution of 11.6 nm. All of these achievements point the way toward high-speed X-ray imaging without lens-imposed resolution limit.

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.

Micro-XRF for characterization of Moroccan glazed ceramics and Portuguese tiles

NASA Astrophysics Data System (ADS)

Guilherme, A.; Manso, M.; Pessanha, S.; Zegzouti, A.; Elaatmani, M.; Bendaoud, R.; Coroado, J.; dos Santos, J. M. F.; Carvalho, M. L.

2013-02-01

A set of enamelled terracotta samples (Zellij) collected from five different monuments in Morocco were object of study. With the aim of characterizing these typically Moroccan artistic objects, X-ray spectroscopic techniques were used as analytical tool to provide elemental and compound information. A lack of information about these types of artistic ceramics is found by the research through international scientific journals, so this investigation is an opportunity to fulfill this gap. For this purpose, micro-Energy Dispersive X-ray Fluorescence (μ-EDXRF), and wavelength dispersive X-ray Fluorescence (WDXRF) and X-ray Diffraction (XRD) were the chosen methods. As complementary information, a comparison with other sort of artistic pottery objects is given, more precisely with Portuguese glazed wall tiles (Azulejos), based in the Islamic pottery traditions. Differences between these two types of decorative pottery were found and presented in this manuscript.

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.

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.

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

X-ray fluorescence camera for imaging of iodine media in vivo.

PubMed

Matsukiyo, Hiroshi; Watanabe, Manabu; Sato, Eiichi; Osawa, Akihiro; Enomoto, Toshiyuki; Nagao, Jiro; Abderyim, Purkhet; Aizawa, Katsuo; Tanaka, Etsuro; Mori, Hidezo; Kawai, Toshiaki; Ehara, Shigeru; Sato, Shigehiro; Ogawa, Akira; Onagawa, Jun

2009-01-01

X-ray fluorescence (XRF) analysis is useful for measuring density distributions of contrast media in vivo. An XRF camera was developed for carrying out mapping for iodine-based contrast media used in medical angiography. Objects are exposed by an X-ray beam from a cerium target. Cerium K-series X-rays are absorbed effectively by iodine media in objects, and iodine fluorescence is produced from the objects. Next, iodine Kalpha fluorescence is selected out by use of a 58-microm-thick stannum filter and is detected by a cadmium telluride (CdTe) detector. The Kalpha rays are discriminated out by 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 iodine mapping are shown on a personal computer monitor. The scan pitch of the x and y axes was 2.5 mm, and the photon counting time per mapping point was 2.0 s. We carried out iodine mapping of non-living animals (phantoms), and iodine Kalpha fluorescence was produced from weakly remaining iodine elements in a rabbit skin cancer.

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.

[Experimental study and correction of the absorption and enhancement effect between Ti, V and Fe].

PubMed

Tuo, Xian-Guo; Mu, Ke-Liang; Li, Zhe; Wang, Hong-Hui; Luo, Hui; Yang, Jian-Bo

2009-11-01

The absorption and enhancement effects in X-ray fluorescence analysis for Ti, V and Fe elements were studied in the present paper. Three bogus duality systems of Ti-V/Ti-Fe/V-Fe samples were confected and measured by X-ray fluorescence analysis technique using HPGe semiconductor detector, and the relation curve between unitary coefficient (R(K)) of element count rate and element content (W(K)) were obtained after the experiment. Having analyzed the degree of absorption and enhancement effect between every two elements, the authors get the result, and that is the absorption and enhancement effect between Ti and V is relatively distinctness, while it's not so distinctness in Ti-Fe and V-Fe. After that, a mathematics correction method of exponential fitting was used to fit the R(K)-W(K) curve and get a function equation of X-ray fluorescence count rate and content. Three groups of Ti-V duality samples were used to test the fitting method and the relative errors of Ti and V were less than 0.2% as compared to the actual results.

Method of loading organic materials with group III plus lanthanide and actinide elements

DOEpatents

Bell, Zane W [Oak Ridge, TN; Huei-Ho, Chuen [Oak Ridge, TN; Brown, Gilbert M [Knoxville, TN; Hurlbut, Charles [Sweetwater, TX

2003-04-08

Disclosed is a composition of matter comprising a tributyl phosphate complex of a group 3, lanthanide, actinide, or group 13 salt in an organic carrier and a method of making the complex. These materials are suitable for use in solid or liquid organic scintillators, as in x-ray absorption standards, x-ray fluorescence standards, and neutron detector calibration standards.

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.

Energy dispersive X-ray fluorescence determination of cadmium in uranium matrix using Cd Kα line excited by continuum

NASA Astrophysics Data System (ADS)

Dhara, Sangita; Misra, N. L.; Aggarwal, S. K.; Venugopal, V.

2010-06-01

An energy dispersive X-ray fluorescence method for determination of cadmium (Cd) in uranium (U) matrix using continuum source of excitation was developed. Calibration and sample solutions of cadmium, with and without uranium were prepared by mixing different volumes of standard solutions of cadmium and uranyl nitrate, both prepared in suprapure nitric acid. The concentration of Cd in calibration solutions and samples was in the range of 6 to 90 µg/mL whereas the concentration of Cd with respect to U ranged from 90 to 700 µg/g of U. From the calibration solutions and samples containing uranium, the major matrix uranium was selectively extracted using 30% tri-n-butyl phosphate in dodecane. Fixed volumes (1.5 mL) of aqueous phases thus obtained were taken directly in specially designed in-house fabricated leak proof Perspex sample cells for the energy dispersive X-ray fluorescence measurements and calibration plots were made by plotting Cd Kα intensity against respective Cd concentration. For the calibration solutions not having uranium, the energy dispersive X-ray fluorescence spectra were measured without any extraction and Cd calibration plots were made accordingly. The results obtained showed a precision of 2% (1 σ) and the results deviated from the expected values by < 4% on average.

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

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

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

Towards a nanoscale mammographic contrast agent: development of a modular pre-clinical dual optical/x-ray agent

NASA Astrophysics Data System (ADS)

Hill, Melissa L.; Gorelikov, Ivan; Niroui, Farnaz; Levitin, Ronald B.; Mainprize, James G.; Yaffe, Martin J.; Rowlands, J. A.; Matsuura, Naomi

2013-08-01

Contrast-enhanced digital mammography (CEDM) can provide improved breast cancer detection and characterization compared to conventional mammography by imaging the effects of tumour angiogenesis. Current small-molecule contrast agents used for CEDM are limited by a short plasma half-life and rapid extravasation into tissue interstitial space. To address these limitations, nanoscale agents that can remain intravascular except at sites of tumour angiogenesis can be used. For CEDM, this agent must be both biocompatible and strongly attenuate mammographic energy x-rays. Nanoscale perfluorooctylbromide (PFOB) droplets have good x-ray attenuation and have been used in patients for other applications. However, the macroscopic scale of x-ray imaging (50-100 µm) is inadequate for direct verification that PFOB droplets localize at sites of breast tumour angiogenesis. For efficient pre-clinical optimization for CEDM, we integrated an optical marker into PFOB droplets for microscopic assessment (≪50 µm). To develop PFOB droplets as a new nanoscale mammographic contrast agent, PFOB droplets were labelled with fluorescent quantum dots (QDs). The droplets had mean diameters of 160 nm, fluoresced at 635 nm and attenuated x-ray spectra at 30.5 keV mean energy with a relative attenuation of 5.6 ± 0.3 Hounsfield units (HU) mg-1 mL-1 QD-PFOB. With the agent loaded into tissue phantoms, good correlation between x-ray attenuation and optical fluorescence was found (R2 = 0.96), confirming co-localization of the QDs with PFOB for quantitative assessment using x-ray or optical methods. Furthermore, the QDs can be removed from the PFOB agent without affecting its x-ray attenuation or structural properties for expedited translation of optimized PFOB droplet formulations into patients.

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.

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.

Element Specific Imaging Using Muonic X-rays

NASA Astrophysics Data System (ADS)

Hillier, Adrian; Ishida, Katsu; Seller, Paul; Veale, Matthew C.; Wilson, Matthew D.

The RIKEN-RAL facility provides a source of negative muons that can be used to non-destructively determine the elemental composition of bulk samples. A negative muon can replace an electron in an atom and subsequently transition to lower orbital positions. As with conventional X-ray fluorescence, an X-ray photon is emitted with a characteristic energy to enable the transition between orbitals of an atom. As the mass of a negative muon is much greater than that of an electron, a higher energy X-ray photon is emitted when the negative muon transitions between orbitals compared to conventional X-ray fluorescence. The higher energy muonic X-rays are able to escape large samples even when they are emitted from lower Z atoms, making muonic X-rays fluorescence a unique method to characterize the elemental content of a sample. In a typical experiment a section of a sample will be probed with negative muons with the muon momentum tuned to interact at a desired depth in the sample. A small number of single element high purity Ge detectors are positioned to capture up to one photon each from each of the forty muon pulses per second at the RIKEN-RAL facility. This can provide a high resolution and high dynamic range X-ray energy spectrum when collected for several hours but can only provide a spatial average or single point elemental distribution per collection. Here, an STFC developed CdTe detector with 80 × 80 energy resolving channels has been used to demonstrate the ability to image the elemental distribution of a test sample. A test sample of C, Al, and Fe2O3 was positioned close to the detector surface and each of the 250 µm pitch pixels recorded a muonic X-ray energy spectrum. Results are presented to show the principal of this new technique and potential improvements to provide higher resolution and larger area elemental imaging using muonic X-rays are discussed.

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

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

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

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

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

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

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.

Exploring interface morphology of a deeply buried layer in periodic multilayer

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

Das, Gangadhar; Srivastava, A. K.; Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in

2016-06-27

Long-term durability of a thin film device is strongly correlated with the nature of interface structure associated between different constituent layers. Synthetic periodic multilayer structures are primarily employed as artificial X-ray Bragg reflectors in many applications, and their reflection efficiency is predominantly dictated by the nature of the buried interfaces between the different layers. Herein, we demonstrate the applicability of the combined analysis approach of the X-ray reflectivity and grazing incidence X-ray fluorescence measurements for the reliable and precise determination of a buried interface structure inside periodic X-ray multilayer structures. X-ray standing wave field (XSW) generated under Bragg reflection conditionmore » is used to probe the different constituent layers of the W- B{sub 4}C multilayer structure at 10 keV and 12 keV incident X-ray energies. Our results show that the XSW assisted fluorescence measurements are markedly sensitive to the location and interface morphology of a buried layer structure inside a periodic multilayer structure. The cross sectional transmission electron microscopy results obtained on the W-B{sub 4}C multilayer structure provide a deeper look on the overall reliability and accuracy of the XSW method. The method described here would also be applicable for nondestructive characterization of a wide range of thin film based semiconductor and optical devices.« less

Incoherent-scatter computed tomography with monochromatic synchrotron x ray: feasibility of multi-CT imaging system for simultaneous measurement-of fluorescent and incoherent scatter x rays

NASA Astrophysics Data System (ADS)

Yuasa, T.; Akiba, M.; Takeda, T.; Kazama, M.; Hoshino, A.; Watanabe, Y.; Hyodo, K.; Dilmanian, F. A.; Akatsuka, T.; Itai, Y.

1997-10-01

We describe a new system of incoherent scatter computed tomography (ISCT) using monochromatic synchrotron X rays, and we discuss its potential to be used in in vivo imaging for medical use. The system operates on the basis of computed tomography (CT) of the first generation. The reconstruction method for ISCT uses the least squares method with singular value decomposition. The research was carried out at the BLNE-5A bending magnet beam line of the Tristan Accumulation Ring in KEK, Japan. An acrylic cylindrical phantom of 20-mm diameter containing a cross-shaped channel was imaged. The channel was filled with a diluted iodine solution with a concentration of 200 /spl mu/gI/ml. Spectra obtained with the system's high purity germanium (HPGe) detector separated the incoherent X-ray line from the other notable peaks, i.e., the iK/sub /spl alpha// and K/sub /spl beta/1/ X-ray fluorescent lines and the coherent scattering peak. CT images were reconstructed from projections generated by integrating the counts In the energy window centering around the incoherent scattering peak and whose width was approximately 2 keV. The reconstruction routine employed an X-ray attenuation correction algorithm. The resulting image showed more homogeneity than one without the attenuation correction.

Chemical imaging analysis of the brain with X-ray methods

NASA Astrophysics Data System (ADS)

Collingwood, Joanna F.; Adams, Freddy

2017-04-01

Cells employ various metal and metalloid ions to augment the structure and the function of proteins and to assist with vital biological processes. In the brain they mediate biochemical processes, and disrupted metabolism of metals may be a contributing factor in neurodegenerative disorders. In this tutorial review we will discuss the particular role of X-ray methods for elemental imaging analysis of accumulated metal species and metal-containing compounds in biological materials, in the context of post-mortem brain tissue. X-rays have the advantage that they have a short wavelength and can penetrate through a thick biological sample. Many of the X-ray microscopy techniques that provide the greatest sensitivity and specificity for trace metal concentrations in biological materials are emerging at synchrotron X-ray facilities. Here, the extremely high flux available across a wide range of soft and hard X-rays, combined with state-of-the-art focusing techniques and ultra-sensitive detectors, makes it viable to undertake direct imaging of a number of elements in brain tissue. The different methods for synchrotron imaging of metals in brain tissues at regional, cellular, and sub-cellular spatial resolution are discussed. Methods covered include X-ray fluorescence for elemental imaging, X-ray absorption spectrometry for speciation imaging, X-ray diffraction for structural imaging, phase contrast for enhanced contrast imaging and scanning transmission X-ray microscopy for spectromicroscopy. Two- and three-dimensional (confocal and tomographic) imaging methods are considered as well as the correlation of X-ray microscopy with other imaging tools.

Elemental Composition of Mars Return Samples Using X-Ray Fluorescence Imaging at the National Synchrotron Light Source II

NASA Astrophysics Data System (ADS)

Thieme, J.; Hurowitz, J. A.; Schoonen, M. A.; Fogelqvist, E.; Gregerson, J.; Farley, K. A.; Sherman, S.; Hill, J.

2018-04-01

NSLS-II at BNL provides a unique and critical capability to perform assessments of the elemental composition and the chemical state of Mars returned samples using synchrotron radiation X-ray fluorescence imaging and X-ray absorption spectroscopy.

Apparatus for monitoring X-ray beam alignment

DOEpatents

Steinmeyer, Peter A.

1991-10-08

A self-contained, hand-held apparatus is provided for minitoring alignment of an X-ray beam in an instrument employing an X-ray source. The apparatus includes a transducer assembly containing a photoresistor for providing a range of electrical signals responsive to a range of X-ray beam intensities from the X-ray beam being aligned. A circuit, powered by a 7.5 VDC power supply and containing an audio frequency pulse generator whose frequency varies with the resistance of the photoresistor, is provided for generating a range of audible sounds. A portion of the audible range corresponds to low X-ray beam intensity. Another portion of the audible range corresponds to high X-ray beam intensity. The transducer assembly may include an a photoresistor, a thin layer of X-ray fluorescent material, and a filter layer transparent to X-rays but opaque to visible light. X-rays from the beam undergoing alignment penetrate the filter layer and excite the layer of fluorescent material. The light emitted from the fluorescent material alters the resistance of the photoresistor which is in the electrical circuit including the audio pulse generator and a speaker. In employing the apparatus, the X-ray beam is aligned to a complete alignment by adjusting the X-ray beam to produce an audible sound of the maximum frequency.

Apparatus for monitoring X-ray beam alignment

DOEpatents

Steinmeyer, P.A.

1991-10-08

A self-contained, hand-held apparatus is provided for monitoring alignment of an X-ray beam in an instrument employing an X-ray source. The apparatus includes a transducer assembly containing a photoresistor for providing a range of electrical signals responsive to a range of X-ray beam intensities from the X-ray beam being aligned. A circuit, powered by a 7.5 VDC power supply and containing an audio frequency pulse generator whose frequency varies with the resistance of the photoresistor, is provided for generating a range of audible sounds. A portion of the audible range corresponds to low X-ray beam intensity. Another portion of the audible range corresponds to high X-ray beam intensity. The transducer assembly may include an a photoresistor, a thin layer of X-ray fluorescent material, and a filter layer transparent to X-rays but opaque to visible light. X-rays from the beam undergoing alignment penetrate the filter layer and excite the layer of fluorescent material. The light emitted from the fluorescent material alters the resistance of the photoresistor which is in the electrical circuit including the audio pulse generator and a speaker. In employing the apparatus, the X-ray beam is aligned to a complete alignment by adjusting the X-ray beam to produce an audible sound of the maximum frequency. 2 figures.

Specimen preparation for x-ray fluorescence analysis of solutions

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

Eksperiandova, L.P.; Spolnik, Z.M.; Blank, A.B.

1995-12-31

Specimens for x-ray fluorescence analysis (XRFA) were prepared by adding dry gelatine (10%) to the analysis solution, homogenizing the mixture and cooling for 20 minutes. Thus, a compact resilient mass could be formed with the required shape and size; the roughness of the surface was determined by the roughness of the surface on which the specimen was formed, much the same as highly polished. Various calibration methods can be applied in the XRFA of a variety of materials if such specimens are used. 12 refs., 1 fig., 2 tabs.

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.

A new anthropometric phantom for calibrating in vivo measurements of stable lead in the human leg using X-ray fluorescence

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

Spitz, H.; Jenkins, M.; Lodwick, J.

2000-02-01

A new anthropometric phantom has been developed for calibrating in vivo measurements of stable lead deposited in bone using x-ray fluorescence. The phantom reproduces the shape of the mid shaft of the adult human leg and is fabricated using polyurethanes and calcium carbonate to produce materials that exhibit the same density, energy transmission, and calcium content as cortical bone, bone marrow, and muscle. The phantom includes a removable tibia fabricated using simulants for cortical bone and bone marrow to which a precise amount of stable lead has been added to cortical bone. The formulations used in fabricating the new anthropometricmore » phantom are much more uniform in density and composition than the conventional phantom made from Plexiglas cylinders filled with plaster-of-Paris. The energy spectrum from an x-ray fluorescence measurement of the phantom using a {sup 109}Cd source is indistinguishable from an in vivo x-ray fluorescence measurement of the human leg, demonstrating that the materials used in the phantom exhibit the same radiological properties as human tissue. Likewise, results from x-ray fluorescence measurements of the phantom exhibit the same positional dependency as the human leg and vary by approximately 36% when, for example, the phantom containing 54 ppm of stable lead in the tibia was rotated by only 15 degrees. The detection limit for a 30 min {sup 109}Cd K shell x-ray fluorescence in vivo measurement is approximately 20 ppm determined from a background measurement using the new phantom containing no added lead in the muscle, bone, or bone marrow. The new anthropometric phantom significantly improves in vivo x-ray fluorescence calibration measurements by (1) faithfully reproducing the anatomy of the human leg, (2) having components that exhibit radiological properties similar to that of human tissue, and (3) providing a realistic calibration standard that can be used for in vivo x-ray fluorescence intercomparison measurements.« less

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

Ice, G.E.; Barbee, T.; Bionta, R.

The increasing availability of synchrotron x-ray sources has stimulated the development of advanced hard x-ray (E{>=}5 keV) microprobes. New x-ray optics have been demonstrated which show promise for achieving intense submicron hard x-ray probes. These probes will be used for extraordinary elemental detection by x-ray fluorescence/absorption and for microdiffraction to identify phase and strain. The inherent elemental and crystallographic sensitivity of an x-ray microprobe and its inherently nondestructive and penetrating nature makes the development of an advanced hard x-ray microprobe an important national goal. In this workshop state-of-the-art hard x-ray microprobe optics were described and future directions were discussed. Genemore » Ice, Oak Ridge National Laboratory (ORNL), presented an overview of the current status of hard x-ray microprobe optics and described the use of crystal spectrometers to improve minimum detectable limits in fluorescent microprobe experiments. Al Thompson, Lawrence Berkeley Laboratory (LBL), described work at the Center for X-ray Optics to develop a hard x-ray microprobe based on Kirkpatrick-Baez (KB) optics. Al Thompson also showed the results of some experimental measurements with their KB optics. Malcolm Howells presented a method for bending elliptical mirrors and Troy Barbee commented on the use of graded d spacings to achieve highest efficiency in KB multilayer microfocusing. Richard Bionta, Lawrence Livermore National Laboratory (LLNL), described the development of the first hard x-ray zone plates and future promise of so called {open_quotes}jelly roll{close_quotes} or sputter slice zone plates. Wenbing Yun, Argonne National Laboratory (ANL), described characterization of jelly roll and lithographically produced zone plates and described the application of zone plates to focus extremely narrow bandwidths by nuclear resonance. This report summarizes the presentations of the workshop subgroup on hard x-ray microprobes.« less

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.

The study of chemical composition and elemental mappings of colored over-glaze porcelain fired in Qing Dynasty by micro-X-ray fluorescence

NASA Astrophysics Data System (ADS)

Lin, Cheng; Meitian, Li; Youshi, Kim; Changsheng, Fan; Shanghai, Wang; Qiuli, Pan; Zhiguo, Liu; Rongwu, Li

2011-02-01

It is very difficult to measure the chemical composition of colored pigments of over-glaze porcelain by X-ray fluorescence because it contains high concentration of Pb. One of the disadvantages of our polycapillary optics is that it has low transmission efficiency to the high energy X-ray. However, it is beneficial to measure the chemical compositions of rich Pb sample. In this paper, we reported the performances of a tabletop setup of micro-X-ray fluorescence system base on slightly focusing polycapillary and its applications for analysis of rich Pb sample. A piece of Chinese ancient over-glaze porcelain was analyzed by micro-X-ray fluorescence. The experimental results showed that the Cu, Fe and Mn are the major color elements. The possibilities of the process of decorative technology were discussed in this paper, also.

ICG-enhanced imaging of arthritis with an integrated Optical Imaging/X-ray System

PubMed Central

Meier, Reinhard; Krug, Christian; Golovko, Daniel; Boddington, Sophie; Piontek, Guido; Rudelius, Martina; Sutton, Elizabeth J.; Baur-Melnyk, Andrea; Jones, Ella F.; Daldrup-Link, Heike E.

2010-01-01

Background Optical Imaging (OI) is a promising technique that is quick, inexpensive and, in combination with Indocyanine Green (ICG), an FDA-approved fluorescent dye, could provide early detection of rheumatoid arthritis. Objective The purpose of this study was to evaluate a combined X-ray/OI imaging system for ICG-enhanced detection of arthritic joints in a rat model of antigen induced arthritis. Methods Arthritis of the knee and ankle joints was induced in six Harlan rats with peptidoglycan polysaccharide polymers (PGPS). Three rats served as non-treated controls. Optical imaging of the knee and ankle joints was done with an integrated OI/X-ray system before and up to 24h post intravenous injection (p.i.) of 10mg/kg ICG. The fluorescence signal intensities of arthritic and normal joints were compared for significant differences using generalized estimation equation models. Specimen of knee and ankle joints were further processed and evaluated by histology. Results ICG provided a significant increase in fluorescence signal of arthritic joints compared to baseline values immediately after administration (p<0.05). The fluorescence signal of arthritic joints was significantly higher compared to the non-arthritic control joints at 1 - 720 min p.i. (p<0.05). Fusion of ICG-enhanced OI and X-rays allowed for anatomical co-registration of the inflamed tissue with the associated joint. H&E stains confirmed marked synovial inflammation of arthritic joints and absence of inflammation in control joints. Conclusion ICG-enhanced OI is a clinically applicable tool for detection of arthritic tissue. Using relatively high doses of ICG, a long term fluorescence enhancement of arthritic joints can be achieved. This may facilitate simultaneous evaluations of multiple joints in a clinical setting. Fusion of ICG-OI scans with X-ray imaging increases anatomical resolution. PMID:20506388

The Mapping X-Ray Fluorescence Spectrometer (mapx)

NASA Astrophysics Data System (ADS)

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

2016-12-01

MapX will provide elemental imaging at ≤100 µm spatial resolution over 2.5 X 2.5 cm areas, yielding elemental chemistry at or below the scale length where many relict physical, chemical, and biological features can be imaged and interpreted in ancient rocks. MapX is a full-frame spectroscopic imager positioned on soil or regolith with touch sensors. During an analysis, an X-ray source (tube or radioisotope) bombards the sample surface with X-rays or α-particles / γ-rays, resulting in sample X-ray Fluorescence (XRF). Fluoresced X-rays pass through an X-ray lens (X-ray µ-Pore Optic, "MPO") that projects a spatially resolved image of the X-rays onto a CCD. The CCD is operated in single photon counting mode so that the positions and energies of individual photons are retained. In a single analysis, several thousand frames are stored and processed. A MapX experiment provides elemental maps having a spatial resolution of ≤100 µm and quantitative XRF spectra from Regions of Interest (ROI) 2 cm ≤ x ≤ 100 µm. ROI are compared with known rock and mineral compositions to extrapolate the data to rock types and putative mineralogies. The MapX geometry is being refined with ray-tracing simulations and with synchrotron experiments at SLAC. Source requirements are being determined through Monte Carlo modeling and experiment using XMIMSIM [1], GEANT4 [2] and PyMca [3] and a dedicated XRF test fixture. A flow-down of requirements for both tube and radioisotope sources is being developed from these experiments. In addition to Mars lander and rover missions, MapX could be used for landed science on other airless bodies (Phobos/Deimos, Comet nucleus, asteroids, the Earth's moon, and the icy satellites of the outer planets, including Europa. [1] Schoonjans, T. et al.(2012). Spectrachim. Acta Part B, 70, 10-23. [2] Agostinelli, S. et al. (2003). Nucl. Instr. and Methods in Phys. Research A, 506, 250-303. [3] V.A. Solé et al. (2007). Spectrochim. Acta Part B, 62, 63-68.

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.

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.

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

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

Kayser, Y., E-mail: yves.kayser@psi.ch; Paul Scherrer Institut, 5232 Villigen-PSI; Błachucki, W.

2014-04-15

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

Imaging performance of a hybrid x-ray computed tomography-fluorescence molecular tomography system using priors.

PubMed

Ale, Angelique; Schulz, Ralf B; Sarantopoulos, Athanasios; Ntziachristos, Vasilis

2010-05-01

The performance is studied of two newly introduced and previously suggested methods that incorporate priors into inversion schemes associated with data from a recently developed hybrid x-ray computed tomography and fluorescence molecular tomography system, the latter based on CCD camera photon detection. The unique data set studied attains accurately registered data of high spatially sampled photon fields propagating through tissue along 360 degrees projections. Approaches that incorporate structural prior information were included in the inverse problem by adding a penalty term to the minimization function utilized for image reconstructions. Results were compared as to their performance with simulated and experimental data from a lung inflammation animal model and against the inversions achieved when not using priors. The importance of using priors over stand-alone inversions is also showcased with high spatial sampling simulated and experimental data. The approach of optimal performance in resolving fluorescent biodistribution in small animals is also discussed. Inclusion of prior information from x-ray CT data in the reconstruction of the fluorescence biodistribution leads to improved agreement between the reconstruction and validation images for both simulated and experimental data.

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.

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.

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.

United States Air Force Summer Research Program -- 1993 Summer Research Program Final Reports. Volume 15. Wright Laboratory

DTIC Science & Technology

1993-01-01

Two other methods were used to determine the quality of the films. One is x - ray diffraction which is used to determine the crystallographic...orientation of the films. No phases other than the YBa 2Cu3O7. x were observed in any of the films. The x - ray data for the films with high critical current...spectra cups. The first analysis was done using the Portable X - ray Fluorescence Spectrometer. The soil samples. as well as. 10 metal fragments that

Measured and calculated K-fluorescence effects on the MTF of an amorphous-selenium based CCD x-ray detector.

PubMed

Hunter, David M; Belev, George; Kasap, Safa; Yaffe, Martin J

2012-02-01

Theoretical reasoning suggests that direct conversion digital x-ray detectors based upon photoconductive amorphous-selenium (a-Se) could attain very high values of the MTF (modulation transfer function) at spatial frequencies well beyond 20 cycles mm(-1). One of the fundamental factors affecting resolution loss, particularly at x-ray energies just above the K-edge of selenium (12.66 keV), is the K-fluorescence reabsorption mechanism, wherein energy can be deposited in the detector at locations laterally displaced from the initial x-ray interaction site. This paper compares measured MTF changes above and below the Se K-edge of a CCD based a-Se x-ray detector with theoretical expectations. A prototype 25 μm sampling pitch (Nyquist frequency = 20 cycles mm(-1), 200 μm thick a-Se layer based x-ray detector, utilizing a specialized CCD readout device (200 × 400 area array), was used to make edge images with monochromatic x-rays above and below the K-edge of Se. A vacuum double crystal monochromator, exposed to polychromatic x-rays from a synchrotron, formed the monochromatic x-ray source. The monochromaticity of the x-rays was 99% or better. The presampling MTF was determined using the slanted edge method. The theory modeling the MTF performance of the detector includes the basic x-ray interaction physics in the a-Se layer as well as effects related to the operation of the CCD and charge trapping at a blocking layer present at the CCD/a-Se interface. The MTF performance of the prototype a-Se CCD was reduced from the theoretical value prescribed by the basic Se x-ray interaction physics, principally by the presence of a blocking layer. Nevertheless, the K-fluorescence reduction in the MTF was observed, approximately as predicted by theory. For the CCD prototype detector, at five cycles mm(-1), there was a 14% reduction of the MTF, from a value of 0.7 below the K-edge of Se, to 0.6 just above the K-edge. The MTF of an a-Se x-ray detector has been measured using monochromatic x-rays above and below the K-edge of selenium. The MTF is poorer above the K-edge by an amount consistent with theoretical expectations.

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

Das, Gangadhar, E-mail: gdas@rrcat.gov.in; Tiwari, M. K.; Singh, A. K.

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

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.

PyXRF: Python-based X-ray fluorescence analysis package

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

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 sized water phantom has been demonstrated for the first time by means of experiments and MC simulations. PMID:25652502

ENVIRONMENTAL TECHNOLOGY VERFICATION REPORT - FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER - TN SPECTRACE, TN 9000 AND TN PB FIELD PORTABLE X-RAY FLOURESCENCE ANALYZERS

EPA Science Inventory

In April 1995, the U.S. Environmental Protection Agency (EPA) sponsored a demonstration of field portable X-ray fluorescence (FPXRF) analyzers. The primary objectives of this demonstration were to evaluate these analyzers for: (1) their analytical performance relative to standar...

Determination of bromine in selected polymer materials by a wavelength-dispersive X-ray fluorescence spectrometric method - Critical thickness problem and solutions

NASA Astrophysics Data System (ADS)

Gorewoda, Tadeusz; Mzyk, Zofia; Anyszkiewicz, Jacek; Charasińska, Jadwiga

2015-04-01

The purpose of this study was to develop an accurate method for the determination of bromine in polymer materials using X-ray fluorescence spectrometry when the thickness of the sample is less than the bromine critical thickness (tc) value. This is particularly important for analyzing compliance with the Restriction of Hazardous Substances Directive. Mathematically and experimentally estimated tc values in polyethylene and cellulose matrixes were up to several millimeters. Four methods were developed to obtain an accurate result. These methods include the addition of an element with a high mass absorption coefficient, the measurement of the total bromine contained in a defined volume of the sample, the exploitation of tube-Rayleigh line intensities and using the Br-Lβ line.

Airborne particulate matter (PM) filter analysis and modeling by total reflection X-ray fluorescence (TXRF) and X-ray standing wave (XSW).

PubMed

Borgese, L; Salmistraro, M; Gianoncelli, A; Zacco, A; Lucchini, R; Zimmerman, N; Pisani, L; Siviero, G; Depero, L E; Bontempi, E

2012-01-30

This work is presented as an improvement of a recently introduced method for airborne particulate matter (PM) filter analysis [1]. X-ray standing wave (XSW) and total reflection X-ray fluorescence (TXRF) were performed with a new dedicated laboratory instrumentation. The main advantage of performing both XSW and TXRF, is the possibility to distinguish the nature of the sample: if it is a small droplet dry residue, a thin film like or a bulk sample. Another advantage is related to the possibility to select the angle of total reflection to make TXRF measurements. Finally, the possibility to switch the X-ray source allows to measure with more accuracy lighter and heavier elements (with a change in X-ray anode, for example from Mo to Cu). The aim of the present study is to lay the theoretical foundation of the new proposed method for airborne PM filters quantitative analysis improving the accuracy and efficiency of quantification by means of an external standard. The theoretical model presented and discussed demonstrated that airborne PM filters can be considered as thin layers. A set of reference samples is prepared in laboratory and used to obtain a calibration curve. Our results demonstrate that the proposed method for quantitative analysis of air PM filters is affordable and reliable without the necessity to digest filters to obtain quantitative chemical analysis, and that the use of XSW improve the accuracy of TXRF analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

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.

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.

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.

Internal standards in fluorescent X-ray spectroscopy1 1 Publication authorized by the Director, U.S. Geological Survey.

USGS Publications Warehouse

Adler, I.; Axelrod, J.M.

1955-01-01

The use of internal standards in the analysis of ores and minerals of widely-varying matrix by means of fluorescent X-ray spectroscopy is frequently the most practical approach. Internal standards correct for absorption and enhancement effects except when an absorption edge falls between the comparison lines or a very strong emission line falls between the absorption edges responsible for the comparison lines. Particle size variations may introduce substantial errors. One method of coping with the particle size problem is grinding the sample with an added abrasive. ?? 1955.

X-ray fluorescence holography studies for a Cu3Au crystal

NASA Astrophysics Data System (ADS)

Dąbrowski, K. M.; Dul, D. T.; Jaworska-Gołąb, T.; Rysz, J.; Korecki, P.

2015-12-01

In this work we show that performing a numerical correction for beam attenuation and indirect excitation allows one to fully restore element sensitivity in the three-dimensional reconstruction of the atomic structure. This is exemplified by a comparison of atomic images reconstructed from holograms measured for ordered and disordered phases of a Cu3Au crystal that clearly show sensitivity to changes in occupancy of the atomic sites. Moreover, the numerical correction, which is based on quantitative methods of X-ray fluorescence spectroscopy, was extended to take into account the influence of a disturbed overlayer in the sample.

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

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

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

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

Fluorescent x-ray computed tomography with synchrotron radiation using fan collimator

NASA Astrophysics Data System (ADS)

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

1996-04-01

We describe a new system of fluorescent x-ray computed tomography applied to image nonradioactive contrast materials in vivo. The system operates on the basis of computed tomography (CT) of the first generation. The experiment was also simulated using the Monte Carlo method. The research was carried out at the BLNE-5A bending-magnet beam line of the Tristan Accumulation Ring in Kek, Japan. An acrylic cylindrical phantom containing five paraxial channels of 5 and 4 mm diameters was imaged. The channels were filled with a diluted iodine-based contrast material, with iodine concentrations of 2 mg/ml and 500 (mu) g/ml. Spectra obtained with the system's high purity germanium (HPGe) detector separated clearly the K(alpha ) and K(beta 1) x-ray fluorescent lines, and the Compton scattering. CT images were reconstructed from projections generated by integrating the counts in these spectral lines. The method had adequate sensitivity and detection power, as shown by the experiment and predicted by the simulations, to show the iodine content of the phantom channels, which corresponded to 1 and 4 (mu) g iodine content per pixel in the reconstructed images.

Determination of carrier yields for neutron activation analysis using energy dispersive X-ray spectrometry

USGS Publications Warehouse

Johnson, R.G.; Wandless, G.A.

1984-01-01

A new method is described for determining carrier yield in the radiochemical neutron activation analysis of rare-earth elements in silicate rocks by group separation. The method involves the determination of the rare-earth elements present in the carrier by means of energy-dispersive X-ray fluorescence analysis, eliminating the need to re-irradiate samples in a nuclear reactor after the gamma ray analysis is complete. Results from the analysis of USGS standards AGV-1 and BCR-1 compare favorably with those obtained using the conventional method. ?? 1984 Akade??miai Kiado??.

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.

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

[Characteristics of specifications of transportable inverter-type X-ray equipment].

PubMed

Yamamoto, Keiichi; Miyazaki, Shigeru; Asano, Hiroshi; Shinohara, Fuminori; Ishikawa, Mitsuo; Ide, Toshinori; Abe, Shinji; Negishi, Toru; Miyake, Hiroyuki; Imai, Yoshio; Okuaki, Tomoyuki

2003-07-01

Our X-ray systems study group measured and examined the characteristics of four transportable inverter-type X-ray equipments. X-ray tube voltage and X-ray tube current were measured with the X-ray tube voltage and the X-ray tube current measurement terminals provided with the equipment. X-ray tube voltage, irradiation time, and dose were measured with a non-invasive X-ray tube voltage-measuring device, and X-ray output was measured by fluorescence meter. The items investigated were the reproducibility and linearity of X-ray output, error of pre-set X-ray tube voltage and X-ray tube current, and X-ray tube voltage ripple percentage. The waveforms of X-ray tube voltage, the X-ray tube current, and fluorescence intensity draw were analyzed using the oscilloscope gram and a personal computer. All of the equipment had a preset error of X-ray tube voltage and X-ray tube current that met JIS standards. The X-ray tube voltage ripple percentage of each equipment conformed to the tendency to decrease when X-ray tube voltage increased. Although the X-ray output reproducibility of system A exceeded the JIS standard, the other systems were within the JIS standard. Equipment A required 40 ms for X-ray tube current to reach the target value, and there was some X-ray output loss because of a trough in X-ray tube current. Owing to the influence of the ripple in X-ray tube current, the strength of the fluorescence waveform rippled in equipments B and C. Waveform analysis could not be done by aliasing of the recording device in equipment D. The maximum X-ray tube current of transportable inverter-type X-ray equipment is as low as 10-20 mA, and the irradiation time of chest X-ray photography exceeds 0.1 sec. However, improvement of the radiophotographic technique is required for patients who cannot move their bodies or halt respiration. It is necessary to make the irradiation time of the equipments shorter for remote medical treatment.

Calculated X-ray Intensities Using Monte Carlo Algorithms: A Comparison to Experimental EPMA Data

NASA Technical Reports Server (NTRS)

Carpenter, P. K.

2005-01-01

Monte Carlo (MC) modeling has been used extensively to simulate electron scattering and x-ray emission from complex geometries. Here are presented comparisons between MC results and experimental electron-probe microanalysis (EPMA) measurements as well as phi(rhoz) correction algorithms. Experimental EPMA measurements made on NIST SRM 481 (AgAu) and 482 (CuAu) alloys, at a range of accelerating potential and instrument take-off angles, represent a formal microanalysis data set that has been widely used to develop phi(rhoz) correction algorithms. X-ray intensity data produced by MC simulations represents an independent test of both experimental and phi(rhoz) correction algorithms. The alpha-factor method has previously been used to evaluate systematic errors in the analysis of semiconductor and silicate minerals, and is used here to compare the accuracy of experimental and MC-calculated x-ray data. X-ray intensities calculated by MC are used to generate a-factors using the certificated compositions in the CuAu binary relative to pure Cu and Au standards. MC simulations are obtained using the NIST, WinCasino, and WinXray algorithms; derived x-ray intensities have a built-in atomic number correction, and are further corrected for absorption and characteristic fluorescence using the PAP phi(rhoz) correction algorithm. The Penelope code additionally simulates both characteristic and continuum x-ray fluorescence and thus requires no further correction for use in calculating alpha-factors.

Normal incidence x-ray mirror for chemical microanalysis

DOEpatents

Carr, M.J.; Romig, A.D. Jr.

1987-08-05

An x-ray mirror for both electron column instruments and micro x-ray fluorescence instruments for making chemical, microanalysis comprises a non-planar mirror having, for example, a spherical reflecting surface for x-rays comprised of a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on a substrate and whose layers have a thickness which is a multiple of the wavelength being reflected. For electron column instruments, the wavelengths of interest lie above 1.5nm, while for x-ray fluorescence instruments, the range of interest is below 0.2nm. 4 figs.

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.

Study on the influence of X-ray tube spectral distribution on the analysis of bulk samples and thin films: Fundamental parameters method and theoretical coefficient algorithms

NASA Astrophysics Data System (ADS)

Sitko, Rafał

2008-11-01

Knowledge of X-ray tube spectral distribution is necessary in theoretical methods of matrix correction, i.e. in both fundamental parameter (FP) methods and theoretical influence coefficient algorithms. Thus, the influence of X-ray tube distribution on the accuracy of the analysis of thin films and bulk samples is presented. The calculations are performed using experimental X-ray tube spectra taken from the literature and theoretical X-ray tube spectra evaluated by three different algorithms proposed by Pella et al. (X-Ray Spectrom. 14 (1985) 125-135), Ebel (X-Ray Spectrom. 28 (1999) 255-266), and Finkelshtein and Pavlova (X-Ray Spectrom. 28 (1999) 27-32). In this study, Fe-Cr-Ni system is selected as an example and the calculations are performed for X-ray tubes commonly applied in X-ray fluorescence analysis (XRF), i.e., Cr, Mo, Rh and W. The influence of X-ray tube spectra on FP analysis is evaluated when quantification is performed using various types of calibration samples. FP analysis of bulk samples is performed using pure-element bulk standards and multielement bulk standards similar to the analyzed material, whereas for FP analysis of thin films, the bulk and thin pure-element standards are used. For the evaluation of the influence of X-ray tube spectra on XRF analysis performed by theoretical influence coefficient methods, two algorithms for bulk samples are selected, i.e. Claisse-Quintin (Can. Spectrosc. 12 (1967) 129-134) and COLA algorithms (G.R. Lachance, Paper Presented at the International Conference on Industrial Inorganic Elemental Analysis, Metz, France, June 3, 1981) and two algorithms (constant and linear coefficients) for thin films recently proposed by Sitko (X-Ray Spectrom. 37 (2008) 265-272).

Monte Carlo simulation of X-ray imaging and spectroscopy experiments using quadric geometry and variance reduction techniques

NASA Astrophysics Data System (ADS)

Golosio, Bruno; Schoonjans, Tom; Brunetti, Antonio; Oliva, Piernicola; Masala, Giovanni Luca

2014-03-01

The simulation of X-ray imaging experiments is often performed using deterministic codes, which can be relatively fast and easy to use. However, such codes are generally not suitable for the simulation of even slightly more complex experimental conditions, involving, for instance, first-order or higher-order scattering, X-ray fluorescence emissions, or more complex geometries, particularly for experiments that combine spatial resolution with spectral information. In such cases, simulations are often performed using codes based on the Monte Carlo method. In a simple Monte Carlo approach, the interaction position of an X-ray photon and the state of the photon after an interaction are obtained simply according to the theoretical probability distributions. This approach may be quite inefficient because the final channels of interest may include only a limited region of space or photons produced by a rare interaction, e.g., fluorescent emission from elements with very low concentrations. In the field of X-ray fluorescence spectroscopy, this problem has been solved by combining the Monte Carlo method with variance reduction techniques, which can reduce the computation time by several orders of magnitude. In this work, we present a C++ code for the general simulation of X-ray imaging and spectroscopy experiments, based on the application of the Monte Carlo method in combination with variance reduction techniques, with a description of sample geometry based on quadric surfaces. We describe the benefits of the object-oriented approach in terms of code maintenance, the flexibility of the program for the simulation of different experimental conditions and the possibility of easily adding new modules. Sample applications in the fields of X-ray imaging and X-ray spectroscopy are discussed. Catalogue identifier: AERO_v1_0 Program summary URL:http://cpc.cs.qub.ac.uk/summaries/AERO_v1_0.html Program obtainable from: CPC Program Library, Queen’s University, Belfast, N. Ireland Licensing provisions: GNU General Public License version 3 No. of lines in distributed program, including test data, etc.: 83617 No. of bytes in distributed program, including test data, etc.: 1038160 Distribution format: tar.gz Programming language: C++. Computer: Tested on several PCs and on Mac. Operating system: Linux, Mac OS X, Windows (native and cygwin). RAM: It is dependent on the input data but usually between 1 and 10 MB. Classification: 2.5, 21.1. External routines: XrayLib (https://github.com/tschoonj/xraylib/wiki) Nature of problem: Simulation of a wide range of X-ray imaging and spectroscopy experiments using different types of sources and detectors. Solution method: XRMC is a versatile program that is useful for the simulation of a wide range of X-ray imaging and spectroscopy experiments. It enables the simulation of monochromatic and polychromatic X-ray sources, with unpolarised or partially/completely polarised radiation. Single-element detectors as well as two-dimensional pixel detectors can be used in the simulations, with several acquisition options. In the current version of the program, the sample is modelled by combining convex three-dimensional objects demarcated by quadric surfaces, such as planes, ellipsoids and cylinders. The Monte Carlo approach makes XRMC able to accurately simulate X-ray photon transport and interactions with matter up to any order of interaction. The differential cross-sections and all other quantities related to the interaction processes (photoelectric absorption, fluorescence emission, elastic and inelastic scattering) are computed using the xraylib software library, which is currently the most complete and up-to-date software library for X-ray parameters. The use of variance reduction techniques makes XRMC able to reduce the simulation time by several orders of magnitude compared to other general-purpose Monte Carlo simulation programs. Running time: It is dependent on the complexity of the simulation. For the examples distributed with the code, it ranges from less than 1 s to a few minutes.

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.

Ionic depletion at the crystalline Gibbs layer of PEG-capped gold nanoparticle brushes at aqueous surfaces

NASA Astrophysics Data System (ADS)

Wang, Wenjie; Zhang, Honghu; Mallapragada, Surya; Travesset, Alex; Vaknin, David

2017-12-01

In situ surface-sensitive x-ray diffraction and grazing incidence x-ray fluorescence spectroscopy (GIXFS) methods are combined to determine the ionic distributions across the liquid/vapor interfaces of thiolated-polyethylene-glycol-capped gold nanoparticle (PEG-AuNP) solutions. Induced by the addition of salts (i.e., Cs2SO4 ) to PEG-AuNPs solutions, two-dimensional hexagonal lattices of PEG-AuNPs form spontaneously at the aqueous surfaces, as is demonstrated by x-ray reflectivity and grazing incidence small-angle x-ray scattering. By taking advantage of element specificity with the GIXFS method, we find that the cation Cs+ concentration at the crystalline film is significantly reduced in parts of the PEG-AuNP film compared with that in the bulk.

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.

Evaluation on determination of iodine in coal by energy dispersive X-ray fluorescence

USGS Publications Warehouse

Wang, B.; Jackson, J.C.; Palmer, C.; Zheng, B.; Finkelman, R.B.

2005-01-01

A quick and inexpensive method of relative high iodine determination from coal samples was evaluated. Energy dispersive X-ray fluorescence (EDXRF) provided a detection limit of about 14 ppm (3 times of standard deviations of the blank sample), without any complex sample preparation. An analytical relative standard deviation of 16% was readily attainable for coal samples. Under optimum conditions, coal samples with iodine concentrations higher than 5 ppm can be determined using this EDXRF method. For the time being, due to the general iodine concentrations of coal samples lower than 5 ppm, except for some high iodine content coal, this method can not effectively been used for iodine determination. More work needed to meet the requirement of determination of iodine from coal samples for this method. Copyright ?? 2005 by The Geochemical Society of Japan.

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.

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.

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

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

Jin, Qiaoling; Vogt, Stefan; Lai, Barry

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

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

DOE PAGES

Jin, Qiaoling; Vogt, Stefan; Lai, Barry; ...

2015-02-23

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

Elemental mapping and microimaging by x-ray capillary optics.

PubMed

Hampai, D; Dabagov, S B; Cappuccio, G; Longoni, A; Frizzi, T; Cibin, G; Guglielmotti, V; Sala, M

2008-12-01

Recently, many experiments have highlighted the advantage of using polycapillary optics for x-ray fluorescence studies. We have developed a special confocal scheme for micro x-ray fluorescence measurements that enables us to obtain not only elemental mapping of the sample but also simultaneously its own x-ray imaging. We have designed the prototype of a compact x-ray spectrometer characterized by a spatial resolution of less than 100 microm for fluorescence and less than 10 microm for imaging. A couple of polycapillary lenses in a confocal configuration together with a silicon drift detector allow elemental studies of extended samples (approximately 3 mm) to be performed, while a CCD camera makes it possible to record an image of the same samples with 6 microm spatial resolution, which is limited only by the pixel size of the camera. By inserting a compound refractive lens between the sample and the CCD camera, we hope to develop an x-ray microscope for more enlarged images of the samples under test.

Rapid Analysis of Copper Ore in Pre-Smelter Head Flow Slurry by Portable X-ray Fluorescence.

PubMed

Burnett, Brandon J; Lawrence, Neil J; Abourahma, Jehad N; Walker, Edward B

2016-05-01

Copper laden ore is often concentrated using flotation. Before the head flow slurry can be smelted, it is important to know the concentration of copper and contaminants. The concentration of copper and other elements fluctuate significantly in the head flow, often requiring modification of the concentrations in the slurry prior to smelting. A rapid, real-time analytical method is needed to support on-site optimization of the smelter feedstock. A portable, handheld X-ray fluorescence spectrometer was utilized to determine the copper concentration in a head flow suspension at the slurry origin. The method requires only seconds and is reliable for copper concentrations of 2.0-25%, typically encountered in such slurries. © The Author(s) 2016.

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

Sato-Tomita, Ayana, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp; Shibayama, Naoya, E-mail: ayana.sato@jichi.ac.jp, E-mail: shibayam@jichi.ac.jp, E-mail: hayashi.koichi@nitech.ac.jp; Okabe, Takahiro

Experimental procedure and setup for obtaining X-ray fluorescence hologram of crystalline metalloprotein samples are described. Human hemoglobin, an α{sub 2}β{sub 2} tetrameric metalloprotein containing the Fe(II) heme active-site in each chain, was chosen for this study because of its wealth of crystallographic data. A cold gas flow system was introduced to reduce X-ray radiation damage of protein crystals that are usually fragile and susceptible to damage. A χ-stage was installed to rotate the sample while avoiding intersection between the X-ray beam and the sample loop or holder, which is needed for supporting fragile protein crystals. Huge hemoglobin crystals (with amore » maximum size of 8 × 6 × 3 mm{sup 3}) were prepared and used to keep the footprint of the incident X-ray beam smaller than the sample size during the entire course of the measurement with the incident angle of 0°-70°. Under these experimental and data acquisition conditions, we achieved the first observation of the X-ray fluorescence hologram pattern from the protein crystals with minimal radiation damage, opening up a new and potential method for investigating the stereochemistry of the metal active-sites in biomacromolecules.« less

Compositional homogeneity and X-ray topographic analyses of CdTe xSe 1-x grown by the vertical Bridgman technique

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

Roy, U. N.; Bolotnikov, A. E.; Camarda, G. S.

2015-02-01

We grew CdTe xSe 1-x crystals with nominal Se concentrations of 5%, 7%, and 10% by the vertical Bridgman technique, and evaluated their compositional homogeneity and structural quality at the NSLS’ X-ray fluorescence and white beam X-ray topography beam lines. Both X-ray fluorescence and photoluminescence mapping revealed very high compositional homogeneity of the CdTe xSe 1-x crystals. Here, we noted that those crystals with higher concentrations of Se were more prone to twinning than those with a lower content. The crystals were fairly free from strains and contained low concentrations of sub-grain boundaries and their networks.

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.

3-D Cellular Ultrastructure Can Be Resolved by X-ray Microscopy | Center for Cancer Research

Cancer.gov

X-ray microscopy (XRM) is more rapid than cryoelectron tomography or super-resolution fluorescence microscopy and could fill an important gap in current technologies used to investigate in situ three-dimensional structure of cells. New XRM methods developed by first author Gerd Schneider, Ph.D., working with James McNally. Ph.D., and a team of colleagues, is capable of

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.

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 measurements of the chemical composition of the final samples (EPMA, various energy-dispersive XRF) will serve as calibration standard for XRF-S. Development is funded by the German Aerospace Agency under grant 50 JR 1303.

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.

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.

ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT - FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER - METOREX, INC. X-MET 920-P AND 940

EPA Science Inventory

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

Fat to muscle ratio measurements with dual energy x-ray absorbtiometry

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

Chen, A.; Luo, J.; Wang, A.

Accurate measurement of the fat-to-muscle ratio in animal model is important for obesity research. In addition, an efficient way to measure the fat to muscle ratio in animal model using dual-energy absorptiometry is presented in this paper. A radioactive source exciting x-ray fluorescence from a target material is used to provide the two x-ray energies needed. The x-rays, after transmitting through the sample, are measured with an energy-sensitive Ge detector. Phantoms and specimens were measured. The results showed that the method was sensitive to the fat to muscle ratios with good linearity. A standard deviation of a few percent inmore » the fat to muscle ratio could be observed with the x-ray dose of 0.001 mGy.« less

Fat to muscle ratio measurements with dual energy x-ray absorbtiometry

DOE PAGES

Chen, A.; Luo, J.; Wang, A.; ...

2015-03-14

Accurate measurement of the fat-to-muscle ratio in animal model is important for obesity research. In addition, an efficient way to measure the fat to muscle ratio in animal model using dual-energy absorptiometry is presented in this paper. A radioactive source exciting x-ray fluorescence from a target material is used to provide the two x-ray energies needed. The x-rays, after transmitting through the sample, are measured with an energy-sensitive Ge detector. Phantoms and specimens were measured. The results showed that the method was sensitive to the fat to muscle ratios with good linearity. A standard deviation of a few percent inmore » the fat to muscle ratio could be observed with the x-ray dose of 0.001 mGy.« less

Simultaneously Synchrotron X-ray Fluorescence and Ptychographic Imaging of Frozen Biological Single Cells

DOE PAGES

Chen, S.; Deng, J.; Nashed, Y. S. G.; ...

2016-07-25

Bionanoprobe (BNP), a hard x-ray fluorescence sample-scanning nanoprobe at the Advanced Photon Source of Argonne National Laboratory, has been used to quantitatively study elemental distributions in biological cells with sub-100 nm spatial resolution and high sensitivity. Cryogenic conditions enable biological samples to be studied in their frozen-hydrated state with both ultrastructure and elemental distributions more faithfully preserved compared to conventional chemical fixation or dehydration methods. Furthermore, radiation damage is reduced in two ways: the diffusion rate of free radicals is decreased at low temperatures; and the sample is embedded in vitrified ice, which reduces mass loss.

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.

Nm-scale spatial resolution x-ray imaging with MLL nanofocusing optics: instrumentational requirements and challenges

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

Nazaretski, E.; Yan, H.; Lauer, K.

2016-08-30

The Hard X-ray Nanoprobe (HXN) beamline at NSLS-II has been designed and constructed to enable imaging experiments with unprecedented spatial resolution and detection sensitivity. The HXN X-ray Microscope is a key instrument for the beamline, providing a suite of experimental capabilities which includes scanning fluorescence, diffraction, differential phase contrast and ptychography utilizing Multilayer Laue Lenses (MLL) and zoneplate (ZP) as nanofocusing optics. In this paper, we present technical requirements for the MLL-based scanning microscope, outline the development concept and present first ~15 x 15 nm 2 spatial resolution x-ray fluorescence images.

Doubly curved mica diffractors and their applications to x-ray microprobe fluorescence and microanalysis

NASA Astrophysics Data System (ADS)

Chen, Zewu

This thesis describes the experimental work in the fabrication of doubly-curved mica diffractors and their applications in monochromatic microprobe x-ray fluorescence analysis and wavelength dispersive spectrometry. Three-dimension focusing of x-rays can be achieved by diffraction from a doubly-curved diffractor. A Johann point-focusing mica diffractor was fabricated for focusing the Cu Kα1 radiation and characterized by using a microfocus x-ray source. The intensity of the focused beam was measured to be 1.01 × 108 photons/s at the focal spot. The spot size of the focused beam was measured by the knife edge scan method. A Cu Kα1 focal spot of 43 μm x 68 μm has been obtained. Monochromatic microprobe x-ray fluorescence (MMXRF) analysis was performed by using the focused Cu Kα1 radiation. The microfocus x-ray source was operated at 30 kV and 0.1 mA. MMXRF spectra of bulk specimens of GaAs, Si, ZnSe, Mg and 40 μm thick Muscovite were recorded with a Si(Li) energy dispersive detector. Exceptional high signal-to-background ratios were observed. Due to the low background, detection limits as low as 1.6 ppm were predicted for a measurement time of 500 s for bulk specimens. The detector background was determined by recording a spectrum from an Fe55 source and was found to be a significant contribution to the total observed background. A wavelength dispersive spectrometer was designed and constructed for the use in a JEOL transmission electron microscope. A logarithmic spiral of revolution diffractor was fabricated and used explored for measurement of Ca concentration in the TEM. Bench tests were carried out by using the microfocus x-ray source. Preliminary data of tests in the TEM indicated that the spectrometer may give better performance than EDS systems previously used.

Theoretical and experimental determination of L -shell decay rates, line widths, and fluorescence yields in Ge

NASA Astrophysics Data System (ADS)

Guerra, M.; Sampaio, J. M.; Madeira, T. I.; Parente, F.; Indelicato, P.; Marques, J. P.; Santos, J. P.; Hoszowska, J.; Dousse, J.-Cl.; Loperetti, L.; Zeeshan, F.; Müller, M.; Unterumsberger, R.; Beckhoff, B.

2015-08-01

Fluorescence yields (FYs) for the Ge L shell were determined by a theoretical and two experimental groups within the framework of the International Initiative on X-Ray Fundamental Parameters Collaboration. Calculations were performed using the Dirac-Fock method, including relativistic and QED corrections. The experimental value of the L3FY ωL 3 was determined at the Physikalisch-Technische Bundesanstalt undulator beamline of the synchrotron radiation facility BESSY II in Berlin, Germany, and the L α1 ,2 and L β1 line widths were measured at the Swiss Light Source, Paul Scherrer Institute, Switzerland, using monochromatized synchrotron radiation and a von Hamos x-ray crystal spectrometer. The measured fluorescence yields and line widths are compared to the corresponding calculated values.

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.

Ionic depletion at the crystalline Gibbs layer of PEG-capped gold nanoparticle brushes at aqueous surfaces

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

Wang, Wenjie; Zhang, Honghu; Mallapragada, Surya

In situ surface-sensitive x-ray diffraction and grazing incidence x-ray fluorescence spectroscopy (GIXFS) methods are combined to determine the ionic distributions across the liquid/vapor interfaces of thiolated-polyethylene-glycol–capped gold nanoparticle (PEG-AuNP) solutions. Induced by the addition of salts (i.e., Cs 2SO 4) to PEG-AuNPs solutions, two-dimensional hexagonal lattices of PEG-AuNPs form spontaneously at the aqueous surfaces, as is demonstrated by x-ray reflectivity and grazing incidence small-angle x-ray scattering. In conclusion, by taking advantage of element specificity with the GIXFS method, we find that the cation Cs + concentration at the crystalline film is significantly reduced in parts of the PEG-AuNP film comparedmore » with that in the bulk.« less

Ionic depletion at the crystalline Gibbs layer of PEG-capped gold nanoparticle brushes at aqueous surfaces

DOE PAGES

Wang, Wenjie; Zhang, Honghu; Mallapragada, Surya; ...

2017-12-14

In situ surface-sensitive x-ray diffraction and grazing incidence x-ray fluorescence spectroscopy (GIXFS) methods are combined to determine the ionic distributions across the liquid/vapor interfaces of thiolated-polyethylene-glycol–capped gold nanoparticle (PEG-AuNP) solutions. Induced by the addition of salts (i.e., Cs 2SO 4) to PEG-AuNPs solutions, two-dimensional hexagonal lattices of PEG-AuNPs form spontaneously at the aqueous surfaces, as is demonstrated by x-ray reflectivity and grazing incidence small-angle x-ray scattering. In conclusion, by taking advantage of element specificity with the GIXFS method, we find that the cation Cs + concentration at the crystalline film is significantly reduced in parts of the PEG-AuNP film comparedmore » with that in the bulk.« less

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

Manohar, Nivedh; Jones, Bernard L.; Cho, Sang Hyun, E-mail: scho@mdanderson.org

Purpose: To develop an accurate and comprehensive Monte Carlo (MC) model of an experimental benchtop polychromatic cone-beam x-ray fluorescence computed tomography (XFCT) setup and apply this MC model to optimize incident x-ray spectrum for improving production/detection of x-ray fluorescence photons from gold nanoparticles (GNPs). Methods: A detailed MC model, based on an experimental XFCT system, was created using the Monte Carlo N-Particle (MCNP) transport code. The model was validated by comparing MC results including x-ray fluorescence (XRF) and scatter photon spectra with measured data obtained under identical conditions using 105 kVp cone-beam x-rays filtered by either 1 mm of leadmore » (Pb) or 0.9 mm of tin (Sn). After validation, the model was used to investigate the effects of additional filtration of the incident beam with Pb and Sn. Supplementary incident x-ray spectra, representing heavier filtration (Pb: 2 and 3 mm; Sn: 1, 2, and 3 mm) were computationally generated and used with the model to obtain XRF/scatter spectra. Quasimonochromatic incident x-ray spectra (81, 85, 90, 95, and 100 keV with 10 keV full width at half maximum) were also investigated to determine the ideal energy for distinguishing gold XRF signal from the scatter background. Fluorescence signal-to-dose ratio (FSDR) and fluorescence-normalized scan time (FNST) were used as metrics to assess results. Results: Calculated XRF/scatter spectra for 1-mm Pb and 0.9-mm Sn filters matched (r ≥ 0.996) experimental measurements. Calculated spectra representing additional filtration for both filter materials showed that the spectral hardening improved the FSDR at the expense of requiring a much longer FNST. In general, using Sn instead of Pb, at a given filter thickness, allowed an increase of up to 20% in FSDR, more prominent gold XRF peaks, and up to an order of magnitude decrease in FNST. Simulations using quasimonochromatic spectra suggested that increasing source x-ray energy, in the investigated range of 81–100 keV, increased the FSDR up to a factor of 20, compared to 1 mm Pb, and further facilitated separation of gold XRF peaks from the scatter background. Conclusions: A detailed MC model of an experimental benchtop XFCT system has been developed and validated. In exemplary calculations to illustrate the usefulness of this model, it was shown that potential use of quasimonochromatic spectra or judicious choice of filter material/thickness to tailor the spectrum of a polychromatic x-ray source can significantly improve the performance of benchtop XFCT, while considering trade-offs between FSDR and FNST. As demonstrated, the current MC model is a reliable and powerful computational tool that can greatly expedite the further development of a benchtop XFCT system for routine preclinical molecular imaging with GNPs and other metal probes.« less

Incoherent Diffractive Imaging via Intensity Correlations of Hard X Rays

NASA Astrophysics Data System (ADS)

Classen, Anton; Ayyer, Kartik; Chapman, Henry N.; Röhlsberger, Ralf; von Zanthier, Joachim

2017-08-01

Established x-ray diffraction methods allow for high-resolution structure determination of crystals, crystallized protein structures, or even single molecules. While these techniques rely on coherent scattering, incoherent processes like fluorescence emission—often the predominant scattering mechanism—are generally considered detrimental for imaging applications. Here, we show that intensity correlations of incoherently scattered x-ray radiation can be used to image the full 3D arrangement of the scattering atoms with significantly higher resolution compared to conventional coherent diffraction imaging and crystallography, including additional three-dimensional information in Fourier space for a single sample orientation. We present a number of properties of incoherent diffractive imaging that are conceptually superior to those of coherent methods.

X-ray excitation fluorescence spectra of the Eu2+-stabilized VK center in alkaline-earth fluoride mixed-crystal systems

NASA Astrophysics Data System (ADS)

Kawano, K.; Ohya, T.; Tsurumi, T.; Katoh, K.; Nakata, R.

1999-11-01

X-ray excitation fluorescence spectra were investigated for MF2:Eu (M=Ca, Sr, and Ba) and their mixed-crystal systems, Ca1-xSrxF2 and Sr1-xBaxF2 with the same fluorite structure. The UV recombination fluorescence band of the VK center associated with blue emission due to the f-d transition of Eu2+ ions was observed with changing mixture ratios x at room temperature. Two sets of weak spectra due to f-f transitions of Eu3+ ions also appeared in the 500-600-nm wavelength region. The peak wavelengths and the integrated intensities of the observed fluorescence were investigated as a function of the Eu concentration as well as the mixture ratio. For the blue emission of Eu2+, pulsed x-ray excitation resulted in shorter lifetimes (500-800 ns) than optical excitation, suggesting energy transfers between the excited states of VK centers and Eu2+. A kinematical fluorescence mechanism was proposed, taking into account the formation of a close pair of a hopping VK center and an immobile Eu2+ ion followed by an energy transfer from the former to the latter. Based on the calculated fluorescence decay curves best fitted to the response curves by x-ray pulse excitation, the energy transfer rates from VK centers to Eu2+ were estimated.

Investigation of molecular mechanisms of action of chelating drugs on protein-lipid model membranes by X-ray fluorescence

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

Novikova, N. N., E-mail: nn_novikova@ns.crys.ras.ru; Zheludeva, S. I.; Koval'chuk, M. V.

Protein-lipid films based on the enzyme alkaline phosphatase were subjected to the action of chelating drugs, which are used for accelerating the removal of heavy metals from the human body, and the elemental composition of the resulting films was investigated. Total-reflection X-ray fluorescence measurements were performed at the Berlin Electron Storage Ring Company for Synchrotron Radiation (BESSY) in Germany. A comparative estimation of the protective effect of four drugs (EDTA, succimer, xydiphone, and mediphon) on membrane-bound enzymes damaged by lead ions was made. The changes in the elemental composition of the protein-lipid films caused by high doses of chelating drugsmore » were investigated. It was shown that state-of-the-art X-ray techniques can, in principle, be used to develop new methods for the in vitro evaluation of the efficiency of drugs, providing differential data on their actions.« less

CARNAÚBA: The Coherent X-Ray Nanoprobe Beamline for the Brazilian Synchrotron SIRIUS/LNLS

NASA Astrophysics Data System (ADS)

Tolentino, Hélio C. N.; Soares, Márcio M.; Perez, Carlos A.; Vicentin, Flávio C.; Abdala, Dalton B.; Galante, Douglas; Teixeira, Verônica de C.; de Araújo, Douglas H. C.; Westfahl, Harry, Jr.

2017-06-01

The CARNAÚBA beamline is the tender-to-hard X-ray (2 - 15 keV) scanning nanoprobe planned for the 4th generation storage ring SIRIUS at the LNLS. CARNAÚBA uses an undulator source with vertical linear polarization in a low-beta straight section and grazing incidence-focusing mirrors to create a nanoprobe at 143 m from the source. The beamline optic is based on KB mirrors and provides high brilliance at an achromatic focal spot down to the diffraction limit diameter of ˜30 nm with a working distance of ˜6 cm. These characteristics are crucial for studying nanometric samples in experiments involving complex stages and environments. The CARNAÚBA beamline aims to perform raster scans using x-ray fluorescence, x-ray absorption spectroscopy, x-ray diffraction and coherent x-ray imaging techniques. Computed tomography will extend these methods to three dimensions.

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.

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.

Use of X-Ray Fluorescence in a Laboratory for the Treatment of Uranium Ores; UTILISATION DE LA FLUORESCENCE DANS UN LABORATOIRE DE TRAITEMENTS DE MINERAIS D'URANIUM

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

Guillet, H.

1960-01-01

A brief description is given of some aspects of the experience gained over a year during which x-ray fluorescence was used at the laberatory of the present Section Autonome d'Etudes, Recherches et Applications Chimiques of the Commissariat a l'Energie Atomique. A standard is tested daily to ensure reproducibility. The observations made during the months from Dec. 1958 to May 1959 are described. In acid leaching of uranium ores, the residues are analyzed by x-ray fluorescence directly in powder form. Fixation and elution of vanadium on ion-exchange resin were also studied. (auth)

Hard x-ray phase contrastmicroscopy - techniques and applications

NASA Astrophysics Data System (ADS)

Holzner, Christian

In 1918, Einstein provided the first description of the nature of the refractive index for X-rays, showing that phase contrast effects are significant. A century later, most x-ray microscopy and nearly all medical imaging remains based on absorption contrast, even though phase contrast offers orders of magnitude improvements in contrast and reduced radiation exposure at multi-keV x-ray energies. The work presented is concerned with developing practical and quantitative methods of phase contrast for x-ray microscopy. A theoretical framework for imaging in phase contrast is put forward; this is used to obtain quantitative images in a scanning microscope using a segmented detector, and to correct for artifacts in a commercial phase contrast x-ray nano-tomography system. The principle of reciprocity between scanning and full-field microscopes is then used to arrive at a novel solution: Zernike contrast in a scanning microscope. These approaches are compared on a theoretical and experimental basis in direct connection with applications using multi-keV x-ray microscopes at the Advanced Photon Source at Argonne National Laboratory. Phase contrast provides the best means to image mass and ultrastructure of light elements that mainly constitute biological matter, while stimulated x-ray fluorescence provides high sensitivity for studies of the distribution of heavier trace elements, such as metals. These approaches are combined in a complementary way to yield quantitative maps of elemental concentration from 2D images, with elements placed in their ultrastructural context. The combination of x-ray fluorescence and phase contrast poses an ideal match for routine, high resolution tomographic imaging of biological samples in the future. The presented techniques and demonstration experiments will help pave the way for this development.

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.

[Simultaneous determination of multiple elements in airborne particulate samples by X-ray fluorescence spectrometry].

PubMed

Takada, T; Hitosugi, M; Kadowaki, T; Kudo, M

1983-07-01

An energy dispersive X-ray fluorescence spectrometer (EDX) has been applied to determine multielements in the workplace air. The standards for X-ray fluorescence analysis were prepared by the chelate precipitation method on polyvinyl chloride (PVC) membrane filter. And, the specimens were prepared to deposit various metal compounds of different chemical forms by the suspension method on PVC membrane filter, and they were determined with EDX and atomic absorption spectrometer (AAS). The results obtained were as follows. Though there is a difference by each element, an amount less than 3 microgram/cm2 per unit area makes it possible to undergo multielement analysis, that is, is has no influence on fine particle effect (particle size; under 5 microns). Then, effects of the X-ray intensity by different chemical forms are negligible. At the presence the neighboring element and other elements this technique showed greater precision by carrying out on corrective treatment, etc. The coefficient of variation of this technique was in the range of 2.5-6.5% at DDTC-Cu of 0.5-5.0 micrograms/cm2, with the limit of detection for As : 0.002 microgram/cm2, Zn : 0.003 microgram/cm2, Pb : 0.003 microgram/cm2, Cu : 0.004 microgram/cm2, Ni : 0.003 microgram/cm2, Fe : 0.005 microgram/cm2, Mn : 0.008 microgram/cm2, Cr : 0.013 microgram/cm2, respectively. Aerosols collected at the workplace were analyzed with EDX and AAS, and the obtained results showed good agreement with such regression line as y = 1.04 chi + 0.04, the coefficient of correlation being r = 0.995. From these results, this technique was found to be a very excellent method for monitoring of multielements in the workplace air.

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.

Growth and luminescent properties of Yb:YAG and Ca co-doped Yb:YAG ultrafast scintillation crystals

NASA Astrophysics Data System (ADS)

Zhu, Maodong; Qi, Hongji; Pan, Mingyan; Hou, Qing; Jiang, Benxue; Jin, Yaxue; Han, Hetong; Song, Zhaohui; Zhang, Hui

2018-05-01

In this work, Yb-doped Y3Al5O12 [yttrium aluminum garnet (YAG)] crystals and Ca co-doped Yb:YAG crystals were grown by the Czochralski (CZ) method. The chemical formulas of the two crystals are (Yb0.1Y0.9)3Al5O12 and (Ca0.001Yb0.1Y0.899)3Al5O12, respectively. The structural, optical and luminescent properties of the Yb:YAG and Ca, Yb:YAG crystals were investigated by X-ray rocking curve, X-ray diffraction, Raman spectra, UV-Visble-NIR absorption spectra and X-ray fluorescence. X-ray fluorescence spectrum with two emission peaks at 330 nm and 490 nm were observed in the two kinds of crystals, which would increase slightly after the annealing. Comparing to the Yb:YAG crystal, Ca co-doped Yb:YAG crystal behaved the better luminescent intensity without changing the crystal structure and vibrational modes. This indicates that by doping Ca2+ in Yb:YAG crystal may be an appropriate way to enhance the luminescent property of the scintillation crystal.

In situ X-ray fluorescence-based method to differentiate among red ochre pigments and yellow ochre pigments thermally transformed to red pigments of wall paintings from Pompeii.

PubMed

Marcaida, Iker; Maguregui, Maite; Fdez-Ortiz de Vallejuelo, Silvia; Morillas, Héctor; Prieto-Taboada, Nagore; Veneranda, Marco; Castro, Kepa; Madariaga, Juan Manuel

2017-06-01

Most of the magnificent wall paintings from the ancient city of Pompeii are decorated with red and yellow colors coming from the ochre pigments used. The thermal impact of the pyroclastic flow from the eruption of Vesuvius, in AD 79, promoted the transformation of some yellow painted areas to red. In this work, original red ochre, original yellow ochre, and transformed yellow ochre (nowadays showing a red color) of wall paintings from Pompeian houses (House of Marcus Lucretius and House of Gilded Cupids) were analyzed by means of a handheld energy-dispersive X-ray fluorescence spectrometer to develop a fast method that allows chemical differentiation of the original red ochre and the transformed yellow ochre. Principal component analysis of the multivariate obtained data showed that arsenic is the tracer element to distinguish between both red colored ochres. Moreover, Pompeian raw red and yellow ochre pigments recovered from the burial were analyzed in the laboratory with use of a benchtop energy-dispersive X-ray fluorescence spectrometer to confirm the elemental composition and the conclusions drawn from the in situ analysis according to the yellow ochre pigment transformation in real Pompeian wall paintings.

Preliminary study on X-ray fluorescence computed tomography imaging of gold nanoparticles: Acceleration of data acquisition by multiple pinholes scheme

NASA Astrophysics Data System (ADS)

Sasaya, Tenta; Sunaguchi, Naoki; Seo, Seung-Jum; Hyodo, Kazuyuki; Zeniya, Tsutomu; Kim, Jong-Ki; Yuasa, Tetsuya

2018-04-01

Gold nanoparticles (GNPs) have recently attracted attention in nanomedicine as novel contrast agents for cancer imaging. A decisive tomographic imaging technique has not yet been established to depict the 3-D distribution of GNPs in an object. An imaging technique known as pinhole-based X-ray fluorescence computed tomography (XFCT) is a promising method that can be used to reconstruct the distribution of GNPs from the X-ray fluorescence emitted by GNPs. We address the acceleration of data acquisition in pinhole-based XFCT for preclinical use using a multiple pinhole scheme. In this scheme, multiple projections are simultaneously acquired through a multi-pinhole collimator with a 2-D detector and full-field volumetric beam to enhance the signal-to-noise ratio of the projections; this enables fast data acquisition. To demonstrate the efficacy of this method, we performed an imaging experiment using a physical phantom with an actual multi-pinhole XFCT system that was constructed using the beamline AR-NE7A at KEK. The preliminary study showed that the multi-pinhole XFCT achieved a data acquisition time of 20 min at a theoretical detection limit of approximately 0.1 Au mg/ml and at a spatial resolution of 0.4 mm.

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.

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...

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...

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.

A Newly Designed Microspectrofluorometer for Kinetic Studies on Protein Crystals in Combination with X-Ray Diffraction

PubMed Central

Klink, Björn U.; Goody, Roger S.; Scheidig, Axel J.

2006-01-01

We present a new design for a fluorescence microspectrophotometer for use in kinetic crystallography in combination with x-ray diffraction experiments. The FLUMIX device (Fluorescence spectroscopy to monitor intermediates in x-ray crystallography) is built for 0° fluorescence detection, which has several advantages in comparison to a conventional fluorometer with 90° design. Due to the reduced spatial requirements and the need for only one objective, the system is highly versatile, easy to handle, and can be used for many different applications. In combination with a conventional stereomicroscope, fluorescence measurements or reaction initiation can be performed directly in a hanging drop crystallization setup. The FLUMIX device can be combined with most x-ray sources, normally without the need of a specialized mechanical support. As a biological model system, we have used H-Ras p21 with an artificially introduced photo-labile GTP precursor (caged GTP) and a covalently attached fluorophore (IANBD amide). Using the FLUMIX system, detailed information about the state of photolyzed crystals of the modified H-Ras p21 (p21(mod)) could be obtained. Measurements in combination with a synchrotron beamline showed significant fluorescence changes in p21(mod) crystals even within a few seconds of x-ray exposure at 100 K. PMID:16698776

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

Identification of heavy metal origins related to chemical and morphological soil properties using several non-destructive X-ray analytical methods.

PubMed

Akbulut, Songul; Grieken, Renevan; Kılıc, Mehmet A; Cevik, Ugur; Rotondo, Giuliana G

2013-03-01

Soils are complex mixtures of organic, inorganic materials, and metal compounds from anthropogenic sources. In order to identify the pollution sources, their magnitude and development, several X-ray analytical methods were applied in this study. The concentrations of 16 elements were determined in all the soil samples using energy dispersive X-ray fluorescence spectrometry. Soils of unknown origin were observed by scanning electron microscopy equipped with a Si(Li) X-ray detector using Monte Carlo simulation approach. The mineralogical analyses were carried out using X-ray diffraction spectrometry. Due to the correlations between heavy metals and oxide compounds, the samples were analyzed also by electron probe microanalyzer (EPMA) in order to have information about their oxide contents. On the other hand, soil pH and salinity levels were identified owing to their influence between heavy metal and soil-surface chemistry. Moreover, the geoaccumulation index (I (geo)) enables the assessment of contamination by comparing current and pre-industrial concentrations.

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

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

PubMed

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

2006-01-01

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

Compression of Born ratio for fluorescence molecular tomography/x-ray computed tomography hybrid imaging: methodology and in vivo validation.

PubMed

Mohajerani, Pouyan; Ntziachristos, Vasilis

2013-07-01

The 360° rotation geometry of the hybrid fluorescence molecular tomography/x-ray computed tomography modality allows for acquisition of very large datasets, which pose numerical limitations on the reconstruction. We propose a compression method that takes advantage of the correlation of the Born-normalized signal among sources in spatially formed clusters to reduce the size of system model. The proposed method has been validated using an ex vivo study and an in vivo study of a nude mouse with a subcutaneous 4T1 tumor, with and without inclusion of a priori anatomical information. Compression rates of up to two orders of magnitude with minimum distortion of reconstruction have been demonstrated, resulting in large reduction in weight matrix size and reconstruction time.

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

PubMed

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

2014-10-01

To develop an accurate and comprehensive Monte Carlo (MC) model of an experimental benchtop polychromatic cone-beam x-ray fluorescence computed tomography (XFCT) setup and apply this MC model to optimize incident x-ray spectrum for improving production/detection of x-ray fluorescence photons from gold nanoparticles (GNPs). A detailed MC model, based on an experimental XFCT system, was created using the Monte Carlo N-Particle (MCNP) transport code. The model was validated by comparing MC results including x-ray fluorescence (XRF) and scatter photon spectra with measured data obtained under identical conditions using 105 kVp cone-beam x-rays filtered by either 1 mm of lead (Pb) or 0.9 mm of tin (Sn). After validation, the model was used to investigate the effects of additional filtration of the incident beam with Pb and Sn. Supplementary incident x-ray spectra, representing heavier filtration (Pb: 2 and 3 mm; Sn: 1, 2, and 3 mm) were computationally generated and used with the model to obtain XRF/scatter spectra. Quasimonochromatic incident x-ray spectra (81, 85, 90, 95, and 100 keV with 10 keV full width at half maximum) were also investigated to determine the ideal energy for distinguishing gold XRF signal from the scatter background. Fluorescence signal-to-dose ratio (FSDR) and fluorescence-normalized scan time (FNST) were used as metrics to assess results. Calculated XRF/scatter spectra for 1-mm Pb and 0.9-mm Sn filters matched (r ≥ 0.996) experimental measurements. Calculated spectra representing additional filtration for both filter materials showed that the spectral hardening improved the FSDR at the expense of requiring a much longer FNST. In general, using Sn instead of Pb, at a given filter thickness, allowed an increase of up to 20% in FSDR, more prominent gold XRF peaks, and up to an order of magnitude decrease in FNST. Simulations using quasimonochromatic spectra suggested that increasing source x-ray energy, in the investigated range of 81-100 keV, increased the FSDR up to a factor of 20, compared to 1 mm Pb, and further facilitated separation of gold XRF peaks from the scatter background. A detailed MC model of an experimental benchtop XFCT system has been developed and validated. In exemplary calculations to illustrate the usefulness of this model, it was shown that potential use of quasimonochromatic spectra or judicious choice of filter material/thickness to tailor the spectrum of a polychromatic x-ray source can significantly improve the performance of benchtop XFCT, while considering trade-offs between FSDR and FNST. As demonstrated, the current MC model is a reliable and powerful computational tool that can greatly expedite the further development of a benchtop XFCT system for routine preclinical molecular imaging with GNPs and other metal probes.

The Mapping X-Ray Fluorescence Spectrometer (MAPX)

NASA Technical Reports Server (NTRS)

Blake, David; Sarrazin, Philippe; Bristow, Thomas; Downs, Robert; Gailhanou, Marc; Marchis, Franck; Ming, Douglas; Morris, Richard; Sole, Vincente Armando; Thompson, Kathleen;

Analytical study of comet nucleus samples

NASA Technical Reports Server (NTRS)

Albee, A. L.

1989-01-01

Analytical procedures for studying and handling frozen (130 K) core samples of comet nuclei are discussed. These methods include neutron activation analysis, x ray fluorescent analysis and high resolution mass spectroscopy.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

NASA Astrophysics Data System (ADS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

Interlaced X-ray diffraction computed tomography

PubMed Central

Vamvakeros, Antonios; Jacques, Simon D. M.; Di Michiel, Marco; Senecal, Pierre; Middelkoop, Vesna; Cernik, Robert J.; Beale, Andrew M.

2016-01-01

An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy. PMID:27047305

Isotopic imaging via nuclear resonance fluorescence with laser-based Thomson radiation

DOEpatents

Barty, Christopher P. J. [Hayward, CA; Hartemann, Frederic V [San Ramon, CA; McNabb, Dennis P [Alameda, CA; Pruet, Jason A [Brentwood, CA

2009-07-21

The present invention utilizes novel laser-based, high-brightness, high-spatial-resolution, pencil-beam sources of spectrally pure hard x-ray and gamma-ray radiation to induce resonant scattering in specific nuclei, i.e., nuclear resonance fluorescence. By monitoring such fluorescence as a function of beam position, it is possible to image in either two dimensions or three dimensions, the position and concentration of individual isotopes in a specific material configuration. Such methods of the present invention material identification, spatial resolution of material location and ability to locate and identify materials shielded by other materials, such as, for example, behind a lead wall. The foundation of the present invention is the generation of quasimonochromatic high-energy x-ray (100's of keV) and gamma-ray (greater than about 1 MeV) radiation via the collision of intense laser pulses from relativistic electrons. Such a process as utilized herein, i.e., Thomson scattering or inverse-Compton scattering, produces beams having diameters from about 1 micron to about 100 microns of high-energy photons with a bandwidth of .DELTA.E/E of approximately 10E.sup.-3.

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 of 170 ng/l of As in xylem sap were achieved.

In vivo tomographic imaging of lung colonization of tumour in mouse with simultaneous fluorescence and X-ray CT.

PubMed

Zhang, Bin; Gao, Fuping; Wang, Mengjiao; Cao, Xu; Liu, Fei; Wang, Xin; Luo, Jianwen; Wang, Guangzhi; Bai, Jing

2014-01-01

Non-invasive in vivo imaging of diffuse and wide-spread colonization within the lungs, rather than distinct solid primary tumors, is still a challenging work. In this work, a lung colonization mouse model bearing A549 human lung tumor was simultaneously scanned by a dual-modality fluorescence molecular tomography (FMT) and X-ray computed tomography (CT) system in vivo. A two steps method which incorporates CT structural information into the FMT reconstruction procedure is employed to provide concurrent anatomical and functional information. By using the target-specific fluorescence agent, the fluorescence tomographic results show elevated fluorescence intensity deep within the lungs which is colonized with diffuse and wide-spread tumors. The results were confirmed with ex vivo fluorescence reflectance imaging and histological examination of the lung tissues. With FMT reconstruction combined with the CT information, the dual-modality FMT/micro-CT system is expected to offer sensitive and noninvasive imaging of diffuse tumor colonization within the lungs in vivo. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Reconstruction method for fluorescent X-ray computed tomography by least-squares method using singular value decomposition

NASA Astrophysics Data System (ADS)

Yuasa, T.; Akiba, M.; Takeda, T.; Kazama, M.; Hoshino, A.; Watanabe, Y.; Hyodo, K.; Dilmanian, F. A.; Akatsuka, T.; Itai, Y.

1997-02-01

We describe a new attenuation correction method for fluorescent X-ray computed tomography (FXCT) applied to image nonradioactive contrast materials in vivo. The principle of the FXCT imaging is that of computed tomography of the first generation. Using monochromatized synchrotron radiation from the BLNE-5A bending-magnet beam line of Tristan Accumulation Ring in KEK, Japan, we studied phantoms with the FXCT method, and we succeeded in delineating a 4-mm-diameter channel filled with a 500 /spl mu/g I/ml iodine solution in a 20-mm-diameter acrylic cylindrical phantom. However, to detect smaller iodine concentrations, attenuation correction is needed. We present a correction method based on the equation representing the measurement process. The discretized equation system is solved by the least-squares method using the singular value decomposition. The attenuation correction method is applied to the projections by the Monte Carlo simulation and the experiment to confirm its effectiveness.

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.

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

NASA Astrophysics Data System (ADS)

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

2014-07-01

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

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.

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.

The Mapping X-ray Fluorescence Spectrometer (MapX)

NASA Astrophysics Data System (ADS)

Sarrazin, P.; Blake, D. F.; Marchis, F.; Bristow, T.; Thompson, K.

2017-12-01

Many planetary surface processes leave traces of their actions as features in the size range 10s to 100s of microns. The Mapping X-ray Fluorescence Spectrometer (MapX) will provide elemental imaging at 100 micron spatial resolution, yielding elemental chemistry at a scale where many relict physical, chemical, or biological features can be imaged and interpreted in ancient rocks on planetary bodies and planetesimals. MapX is an arm-based instrument positioned on a rock or regolith with touch sensors. During an analysis, an X-ray source (tube or radioisotope) bombards the sample with X-rays or alpha-particles / gamma-rays, resulting in sample X-ray Fluorescence (XRF). X-rays emitted in the direction of an X-ray sensitive CCD imager pass through a 1:1 focusing lens (X-ray micro-pore Optic (MPO)) that projects a spatially resolved image of the X-rays onto the CCD. The CCD is operated in single photon counting mode so that the energies and positions of individual X-ray photons are recorded. In a single analysis, several thousand frames are both stored and processed in real-time. Higher level data products include single-element maps with a lateral spatial resolution of 100 microns and quantitative XRF spectra from ground- or instrument- selected Regions of Interest (ROI). XRF spectra from ROI are compared with known rock and mineral compositions to extrapolate the data to rock types and putative mineralogies. When applied to airless bodies and implemented with an appropriate radioisotope source for alpha-particle excitation, MapX will be able to analyze biogenic elements C, N, O, P, S, in addition to the cations of the rock-forming elements >Na, accessible with either X-ray or gamma-ray excitation. The MapX concept has been demonstrated with a series of lab-based prototypes and is currently under refinement and TRL maturation.

Imaging of pharmacokinetic rates of indocyanine green in mouse liver with a hybrid fluorescence molecular tomography/x-ray computed tomography system.

PubMed

Zhang, Guanglei; Liu, Fei; Zhang, Bin; He, Yun; Luo, Jianwen; Bai, Jing

2013-04-01

Pharmacokinetic rates have the potential to provide quantitative physiological and pathological information for biological studies and drug development. Fluorescence molecular tomography (FMT) is an attractive imaging tool for three-dimensionally resolving fluorophore distribution in small animals. In this letter, pharmacokinetic rates of indocyanine green (ICG) in mouse liver are imaged with a hybrid FMT and x-ray computed tomography (XCT) system. A recently developed FMT method using structural priors from an XCT system is adopted to improve the quality of FMT reconstruction. In the in vivo experiments, images of uptake and excretion rates of ICG in mouse liver are obtained, which can be used to quantitatively evaluate liver function. The accuracy of the results is validated by a fiber-based fluorescence measurement system.

Microwave Assisted Synthesis, Physicochemical, Photophysical, Single Crystal X-ray and DFT Studies of Novel Push-Pull Chromophores.

PubMed

Khan, Salman A; Asiri, Abdullah M; Basisi, Hadi Mussa; Arshad, Muhammad Nadeem; Sharma, Kamlesh

2015-11-01

Two push-pull chromophores were synthesized by knoevenagel condensation under microwave irradiation. The structure of synthesized chromophores were established by spectroscopic (FT-IR, (1)H NMR, (13)C NMR, EI-MS) and elemental analysis. Structure of the chromophores was further conformed by X-ray crystallographic. UV-Vis and fluorescence spectroscopy measurements provided that chromophores were good absorbent and fluorescent properties. Fluorescence polarity studies demonstrated that chromophores were sensitive to the polarity of the microenvironment provided by different solvents. Physicochemical parameters, including singlet absorption, extinction coefficient, stokes shift, oscillator strength, dipole moment and flurescence quantum yield were investigated in order to explore the analytical potential of the synthesized chromophores. In addition, the total energy, frontier molecular orbitals, hardness, electron affinity, ionization energy, electrostatic potential map were also studied computationally by using density functional theoretical method.

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.

Demonstration of the feasibility of an integrated x ray laboratory for planetary exploration

NASA Technical Reports Server (NTRS)

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

1993-01-01

The identification of minerals and elemental compositions is an important component in the geological and exobiological exploration of the solar system. X ray diffraction and fluorescence are common techniques for obtaining these data. The feasibility of combining these analytical techniques in an integrated x ray laboratory compatible with the volume, mass, and power constraints imposed by many planetary missions was demonstrated. Breadboard level hardware was developed to cover the range of diffraction lines produced by minerals, clays, and amorphous; and to detect the x ray fluorescence emissions of elements from carbon through uranium. These breadboard modules were fabricated and used to demonstrate the ability to detect elements and minerals. Additional effort is required to establish the detection limits of the breadboard modules and to integrate diffraction and fluorescence techniques into a single unit. It was concluded that this integrated x ray laboratory capability will be a valuable tool in the geological and exobiological exploration of the solar system.

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.

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

Lead foil in dental X-ray film: Backscattering rejection or image intensifier?

NASA Astrophysics Data System (ADS)

Hönnicke, M. G.; Delben, G. J.; Godoi, W. C.; Swinka-Filho, V.

2014-11-01

Dental X-ray films are still largely used due to sterilization issues, simplicity and, mainly, economic reasons. These films almost always are double coated (double emulsion) and have a lead foil in contact with the film for X-ray backscattering rejection. Herein we explore the use of the lead foil as an image intensifier. In these studies, spatial resolution was investigated when images were acquired on the dental X-ray films with and without the lead foil. Also, the lead foil was subjected to atomic analysis (fluorescent measurements) and structure analysis (X-ray diffraction). We determined that the use of the lead foil reduces the exposure time, however, does not affect the spatial resolution on the acquired images. This suggests that the fluorescent radiation spread is smaller than the grain sizes of the dental X-ray films.

ZnO:Gd nanocrystals for fluorescent applications

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

Divya, N. K., E-mail: divyank90@gmail.com; Pradyumnan, P. P.

2016-05-23

Gadolinium doped ZnO crystals within the solubility limit of gadolinium in ZnO matrix were prepared by solid state reaction technique. The method is relatively less expense and enables the production in large scale. The samples were characterised by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), UV/Vis diffuse reflectance spectroscopy and photoluminescence techniques. Fluorescent property studies of gadolinium doped ZnO at room temperature show enhanced visible light emission due to the defects and oxygen vacancies produced via doping. This work reports the impact of gadolinium doping in the structural, optical and luminescent properties of ZnO inmore » detail.« less

Application of instrumental neutron activation and X-ray fluorescence analysis to the examination of objects of art

NASA Astrophysics Data System (ADS)

Panczyk, E.; Ligeza, M.; Walis, L.

1999-01-01

In the Institute of Nuclear Chemistry and Technology in Warsaw in collaboration with the Department of Preservation and Restoration of Works of Art of the Academy of Fine Arts in Cracow and National Museum in Warsaw systematic studies using nuclear methods, particulary instrumental neutron activation analysis and X-ray fluorescence analysis, have been carried out on the panel paintings from the Krakowska- Nowosadecka School and Silesian School of the period from the XIV-XVII century, Chinese and Thai porcelains and mummies fillings of Egyptian sarcophagi. These studies will provide new data to the existing data base, will permit to compare materials used by various schools and individual artists.

Determination of thorium by fluorescent x-ray spectrometry

USGS Publications Warehouse

Adler, I.; Axelrod, J.M.

1955-01-01

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

High-temperature oxidation of advanced FeCrNi alloy in steam environments

NASA Astrophysics Data System (ADS)

Elbakhshwan, Mohamed S.; Gill, Simerjeet K.; Rumaiz, Abdul K.; Bai, Jianming; Ghose, Sanjit; Rebak, Raul B.; Ecker, Lynne E.

2017-12-01

Alloys of iron-chromium-nickel are being explored as alternative cladding materials to improve safety margins under severe accident conditions. Our research focuses on non-destructively investigating the oxidation behavior of the FeCrNi alloy "Alloy 33" using synchrotron-based methods. The evolution and structure of oxide layer formed in steam environments were characterized using X-ray diffraction, hard X-ray photoelectron spectroscopy, X-ray fluorescence methods and scanning electron microscopy. Our results demonstrate that a compact and continuous oxide scale was formed consisting of two layers, chromium oxide and spinel phase (FeCr2O4) oxides, wherein the concentration of the FeCr2O4 phase decreased from the surface to the bulk-oxide interface.

[Rapid determination of major and trace elements in the salt lake clay minerals by X-ray fluorescence spectrometry].

PubMed

Wang, Xiao-Huan; Meng, Qing-Fen; Dong, Ya-Ping; Chen, Mei-Da; Li, Wu

2010-03-01

A rapid multi-element analysis method for clay mineral samples was described. This method utilized a polarized wave-length dispersive X-ray fluorescence spectrometer--Axios PW4400, which had a maximum tube power of 4 000 watts. The method was developed for the determination of As, Mn, Co, Cu, Cr, Dy, Ga, Mo, P, Pb, Rb, S, Sr, Ni, ,Cs, Ta, Th, Ti, U, V, Y, Zn, Zr, MgO, K2O, Na2O, CaO, Fe2O3, Al2O3, SiO2 and so on. Thirty elements in clay mineral species were measured by X-ray fluorescence spectrometry with pressed powder pellets. Spectral interferences, in particular the indirect interferences of each element, were studied. A method to distinguish the interference between each other periodic elements in element periodic table was put forward. The measuring conditions and existence were mainly investigated, and the selected background position as well as corrected spectral overlap for the trace elements were also discussed. It was found that the indirect spectral overlap line was the same important as direct spectral overlap line. Due to inducing the effect of indirect spectral overlap, some elements jlike Bi, Sn, W which do not need analysis were also added to the elements channel. The relative standard deviation (RSD) was in the range of 0.01% to 5.45% except three elements Mo, Cs and Ta. The detection limits, precisions and accuracies for most elements using this method can meet the requirements of sample analysis in clay mineral species.

Optically detected X-ray absorption spectroscopy measurements as a means of monitoring corrosion layers on copper.

PubMed

Dowsett, Mark G; Adriaens, Annemie; Jones, Gareth K C; Poolton, Nigel; Fiddy, Steven; Nikitenko, Sergé

2008-11-15

XANES and EXAFS information is conventionally measured in transmission through the energy-dependent absorption of X-rays or by observing X-ray fluorescence, but secondary fluorescence processes, such as the emission of electrons and optical photons (e.g., 200-1000 nm), can also be used as a carrier of the XAS signatures, providing complementary information such as improved surface specificity. Where the near-visible photons have a shorter range in a material, the data will be more surface specific. Moreover, optical radiation may escape more readily than X-rays through liquid in an environmental cell. Here, we describe a first test of optically detected X-ray absorption spectroscopy (ODXAS) for monitoring electrochemical treatments on copper-based alloys, for example, heritage metals. Artificially made corrosion products deposited on a copper substrate were analyzed in air and in a 1% (w/v) sodium sesquicarbonate solution to simulate typical conservation methods for copper-based objects recovered from marine environments. The measurements were made on stations 7.1 and 9.2 MF (SRS Daresbury, UK) using the mobile luminescence end station (MoLES), supplemented by XAS measurements taken on DUBBLE (BM26 A) at the ESRF. The ODXAS spectra usually contain fine structure similar to that of XAS spectra measured in X-ray fluorescence. Importantly, for the compounds examined, the ODXAS is significantly more surface specific, and >98% characteristic of thin surface layers of 0.5-1.5-microm thickness in cases where X-ray measurements are dominated by the substrate. However, EXAFS and XANES from broadband optical measurements are superimposed on a high background due to other optical emission modes. This produces statistical fluctuations up to double what would be expected from normal counting statistics because the data retain the absolute statistical fluctuation in the original raw count, while losing up to 70% of their magnitude when background is removed. The problem may be solved in future through optical filtering to isolate the information-containing band, combined with the use of higher input X-ray fluxes available on third-generation light sources.

Soft X-Ray Emissions from Planets and Moons

NASA Technical Reports Server (NTRS)

Bhardwaj, A.; Gladstone, G. R.; Elsner, R. F.; Waite, J. H., Jr.; Grodent, D.; Lewis, W. S.; Crary, F. J.; Weisskopf, M. C.; Howell, R. R.; Johnson, R. E.;

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%.

Measurement techniques for trace metals in coal-plant effluents: A brief review

NASA Technical Reports Server (NTRS)

Singh, J. J.

1979-01-01

The strong features and limitations of techniques for determining trace elements in aerosols emitted from coal plants are discussed. Techniques reviewed include atomic absorption spectroscopy, charged particle scattering and activation, instrumental neutron activation analysis, gas/liquid chromatography, gas chromatographic/mass spectrometric methods, X-ray fluorescence, and charged-particle-induced X-ray emission. The latter two methods are emphasized. They provide simultaneous, sensitive multielement analyses and lend themselves readily to depth profiling. It is recommended that whenever feasible, two or more complementary techniques should be used for analyzing environmental samples.

Morphology and dispersion of FeCo alloy nanoparticles dispersed in a matrix of IR pyrolized polyvinyl alcohol

NASA Astrophysics Data System (ADS)

Vasilev, A. A.; Dzidziguri, E. L.; Muratov, D. G.; Zhilyaeva, N. A.; Efimov, M. N.; Karpacheva, G. P.

2018-04-01

Metal-carbon nanocomposites consisting of FeCo alloy nanoparticles dispersed in a carbon matrix were synthesized by the thermal decomposition method of a precursor based on polyvinyl alcohol and metals salts. The synthesized powders were investigated by X-ray diffraction (XRD), X-ray fluorescent spectrometry (XRFS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Surface characteristics of materials were measured by BET-method. The morphology and dispersity of metal nanoparticles were studied depending on the metals ratio in the composite.

Non-Noble Metal Oxide Catalysts for Methane Catalytic Combustion: Sonochemical Synthesis and Characterisation

PubMed Central

Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

2017-01-01

The aim of this study was to obtain nanocrystalline mixed metal-oxide–ZrO2 catalysts via a sonochemically-induced preparation method. The effect of a stabiliser’s addition on the catalyst parameters was investigated by several characterisation methods including X-ray Diffraction (XRD), nitrogen adsorption, X-ray fluorescence (XRF), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), transmission electron microscopy (TEM) and µRaman. The sonochemical preparation method allowed us to manufacture the catalysts with uniformly dispersed metal-oxide nanoparticles at the support surface. The catalytic activity was tested in a methane combustion reaction. The activity of the catalysts prepared by the sonochemical method was higher than that of the reference catalysts prepared by the incipient wetness method without ultrasonic irradiation. The cobalt and chromium mixed zirconia catalysts revealed their high activities, which are comparable with those presented in the literature. PMID:28686190

A new on-axis micro-spectrophotometer for combining Raman, fluorescence and UV/Vis absorption spectroscopy with macromolecular crystallography at the Swiss Light Source

PubMed Central

Pompidor, Guillaume; Dworkowski, Florian S. N.; Thominet, Vincent; Schulze-Briese, Clemens; Fuchs, Martin R.

2013-01-01

The combination of X-ray diffraction experiments with optical methods such as Raman, UV/Vis absorption and fluorescence spectroscopy greatly enhances and complements the specificity of the obtained information. The upgraded version of the in situ on-axis micro-spectrophotometer, MS2, at the macromolecular crystallography beamline X10SA of the Swiss Light Source is presented. The instrument newly supports Raman and resonance Raman spectroscopy, in addition to the previously available UV/Vis absorption and fluorescence modes. With the recent upgrades of the spectral bandwidth, instrument stability, detection efficiency and control software, the application range of the instrument and its ease of operation were greatly improved. Its on-axis geometry with collinear X-ray and optical axes to ensure optimal control of the overlap of sample volumes probed by each technique is still unique amongst comparable facilities worldwide and the instrument has now been in general user operation for over two years. PMID:23955041

A new on-axis micro-spectrophotometer for combining Raman, fluorescence and UV/Vis absorption spectroscopy with macromolecular crystallography at the Swiss Light Source.

PubMed

Pompidor, Guillaume; Dworkowski, Florian S N; Thominet, Vincent; Schulze-Briese, Clemens; Fuchs, Martin R

2013-09-01

The combination of X-ray diffraction experiments with optical methods such as Raman, UV/Vis absorption and fluorescence spectroscopy greatly enhances and complements the specificity of the obtained information. The upgraded version of the in situ on-axis micro-spectrophotometer, MS2, at the macromolecular crystallography beamline X10SA of the Swiss Light Source is presented. The instrument newly supports Raman and resonance Raman spectroscopy, in addition to the previously available UV/Vis absorption and fluorescence modes. With the recent upgrades of the spectral bandwidth, instrument stability, detection efficiency and control software, the application range of the instrument and its ease of operation were greatly improved. Its on-axis geometry with collinear X-ray and optical axes to ensure optimal control of the overlap of sample volumes probed by each technique is still unique amongst comparable facilities worldwide and the instrument has now been in general user operation for over two years.

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

EPA Science Inventory

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

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

EPA Science Inventory

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

Publications - GMC 265 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 265 Publication Details Title: X-ray fluorescence trace element data of the U.S. Bureau of Clautice, K.H., 1996, X-ray fluorescence trace element data of the U.S. Bureau of Mines Idaho Gulch (Tofty

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

EPA Science Inventory

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

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 within subcentimeter-sized ex vivo samples and superficial tumors during preclinical animal studies. PMID:23927295

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

NASA Astrophysics Data System (ADS)

Tellería Narvaez, C. A.; Fernández Alcázar, S.; Barrientos Zamora, F. G.; Chungara Castro, J.; Luna Lauracia, I.; Mamani Tola, H.; Mita Peralta, E.; Muñoz Gosálvez, A. O.; Romero Bolaños, L. E.; Ramírez Ávila, G. M.

2014-06-01

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

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.

Imaging of intracellular fatty acids by scanning X-ray fluorescence microscopy

PubMed Central

Shimura, Mari; Shindou, Hideo; Szyrwiel, Lukasz; Tokuoka, Suzumi M.; Hamano, Fumie; Matsuyama, Satoshi; Okamoto, Mayumi; Matsunaga, Akihiro; Kita, Yoshihiro; Ishizaka, Yukihito; Yamauchi, Kazuto; Kohmura, Yoshiki; Lobinski, Ryszard; Shimizu, Isao; Shimizu, Takao

2016-01-01

Fatty acids are taken up by cells and incorporated into complex lipids such as neutral lipids and glycerophospholipids. Glycerophospholipids are major constituents of cellular membranes. More than 1000 molecular species of glycerophospholipids differ in their polar head groups and fatty acid compositions. They are related to cellular functions and diseases and have been well analyzed by mass spectrometry. However, intracellular imaging of fatty acids and glycerophospholipids has not been successful due to insufficient resolution using conventional methods. Here, we developed a method for labeling fatty acids with bromine (Br) and applied scanning X-ray fluorescence microscopy (SXFM) to obtain intracellular Br mapping data with submicrometer resolution. Mass spectrometry showed that cells took up Br-labeled fatty acids and metabolized them mainly into glycerophospholipids in CHO cells. Most Br signals observed by SXFM were in the perinuclear region. Higher resolution revealed a spot-like distribution of Br in the cytoplasm. The current method enabled successful visualization of intracellular Br-labeled fatty acids. Single-element labeling combined with SXFM technology facilitates the intracellular imaging of fatty acids, which provides a new tool to determine dynamic changes in fatty acids and their derivatives at the single-cell level.—Shimura, M., Shindou, H., Szyrwiel, L., Tokuoka, S. M., Hamano, F., Matsuyama, S., Okamoto, M., Matsunaga, A., Kita, Y., Ishizaka, Y., Yamauchi, K., Kohmura, Y., Lobinski, R., Shimizu, I., Shimizu, T. Imaging of intracellular fatty acids by scanning X-ray fluorescence microscopy. PMID:27601443

GCR-Induced Photon Luminescence of the Moon

NASA Technical Reports Server (NTRS)

Lee, K. T.; Wilson, T. L.

2008-01-01

It is shown that the Moon has a ubiquitous photon luminescence induced by Galactic cosmic-rays (GCRs), using the Monte Carlo particle-physics program FLUKA. Both the fluence and the flux of the radiation can be determined by this method, but only the fluence will be presented here. This is in addition to thermal radiation emitted due to the Moon s internal temperature and radioactivity. This study is a follow-up to an earlier discussion [1] that addressed several misconceptions regarding Moonshine in the Earth-Moon system (Figure 1) and predicted this effect. There also exists a related x-ray fluorescence induced by solar energetic particles (SEPs, <350 MeV) and solar photons at lower x-ray energies, although this latter fluorescence was studied on Apollo 15 and 16 [2- 5], Lunar Prospector [6], and even EGRET [7].

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

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.

Advances in the detection of as in environmental samples using low energy X-ray fluorescence in a scanning transmission X-ray microscope: arsenic immobilization by an Fe(II)-oxidizing freshwater bacteria.

PubMed

Hitchcock, A P; Obst, M; Wang, J; Lu, Y S; Tyliszczak, T

2012-03-06

Speciation and quantitative mapping of elements, organic and inorganic compounds, and mineral phases in environmental samples at high spatial resolution is needed in many areas of geobiochemistry and environmental science. Scanning transmission X-ray microscopes (STXMs) provide a focused beam which can interrogate samples at a fine spatial scale. Quantitative chemical information can be extracted using the transmitted and energy-resolved X-ray fluorescence channels simultaneously. Here we compare the relative merits of transmission and low-energy X-ray fluorescence detection of X-ray absorption for speciation and quantitative analysis of the spatial distribution of arsenic(V) within cell-mineral aggregates formed by Acidovorax sp. strain BoFeN1, an anaerobic nitrate-reducing Fe(II)-oxidizing β-proteobacteria isolated from the sediments of Lake Constance. This species is noted to be highly tolerant to high levels of As(V). Related, As-tolerant Acidovorax-strains have been found in As-contaminated groundwater wells in Bangladesh and Cambodia wherein they might influence the mobility of As by providing sorption sites which might have different properties as compared to chemically formed Fe-minerals. In addition to demonstrating the lower detection limits that are achieved with X-ray fluorescence relative to transmission detection in STXM, this study helps to gain insights into the mechanisms of As immobilization by biogenic Fe-mineral formation and to further the understanding of As-resistance of anaerobic Fe(II)-oxidizing bacteria.

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.

X-ray biosignature of bacteria in terrestrial and extra-terrestrial rocks

NASA Astrophysics Data System (ADS)

Lemelle, L.; Simionovici, A.; Susini, J.; Oger, P.; Chukalina, M.; Rau, Ch.; Golosio, B.; Gillet, P.

2003-04-01

X-ray imaging techniques at the best spatial resolution and using synchrotron facilities are put forth as powerful techniques for the search of small life forms in extraterrestrial rocks under quarantine conditions (Lemelle et al. 2003). Samples, which may be collected in situ on the martian surface or on a cometary surface, will be brought back and finally stored in a container. We tested on the ID22 beamline, the possibilities of the X-ray absorption and fluorescence tomographies on sub-mm grains of NWA817 (Lemelle et al. submitted) and Tatahouine (Simionovici et al. 2001) meteorites stored in a 10 micrometer silica capillary, full of air, mimicking such containers. Studies of the X-ray microtomographies carried on reveal the positions, the 3D textures and mineralogies of the microenvironments where traces of life should be looked for in priority (with a submicrometer spatial resolution). Limitations with respect to bacterial detection are due to the difficulties to obtain information about light elements (Z <= 14), major constituents of biological and silicate samples. At this stage, traces of life were not detected, nor identified such as, on all the studied meteorites through the capillary. Theoretical developments of an internal elemental microanalysis combining X-ray fluorescence, Compton and Transmission tomographies will soon allow improvements of 3D detection of life by X-ray techniques (Golosio et al. submitted). We tested on the ID21 beamline, the possibilities of the X-ray imaging techniques on bacteria/silicate assemblages prepared in the laboratory and directly placed in the beam. The X-ray signature of a "present" bacteria on a silicate surface was defined by X-ray mapping, out of a container, as coincident micrometer and oval zones having strong P and S fluorescence lines (S-fluorescence being slightly lower than P-fluorescence) and an amino-linked sulfur redox speciation. The X-ray signature of a single bacteria can now be applied to test the bacterial origin of nanostructures observed on some meteorite surfaces. Lemelle et al. (2003a) accepted to Journal de Physique, b submitted to Am. Min., Simionovici et al. (2001) Proc. SPIE, vol 4503, ed. U. BONSE, San Diego, August. Golosio et al. submitted to Phys. Rev. B

Measuring and interpreting X-ray fluorescence from planetary surfaces.

PubMed

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

2008-11-15

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

Observational Conditions for the Detection of X-Ray Fluorescence from Sodium by the MIXS Instrument on BepiColombo

NASA Astrophysics Data System (ADS)

Cooper, R.; Grande, M.; Martindale, A.; Bunce, E.

2018-05-01

We model the expected fluorescence from the exosphere and surface of Mercury, as observed by the Mercury Imaging X-ray Spectrometer (MIXS) on the upcoming BepiColombo mission, using code modified from that used for the SMART-1 D-CIXS instrument.

FIELD MEASUREMENT TECHNOLOGY FOR MERCURY IN SOIL AND SEDIMENT NITON'S XLI/XLT 700 SERIES X-RAY FLUORESCENCE ANALYZER

EPA Science Inventory

NITON's XL-700 Series X-ray fluorescence analyzers were demonstrated under the U.S. Environmental Protection Agency Superfund Innovative Technology Evaluation Program in May 2003 at the Oak Ridge National Laboratory (ORNL) in Oak Ridge, Tennessee. The purpose of the Demonstration...

Correlative cryogenic tomography of cells using light and soft x-rays

PubMed Central

Smith, Elizabeth A.; Cinquin, Bertrand P.; Do, Myan; McDermott, Gerry; Le Gros, Mark A.; Larabell, Carolyn A.

2013-01-01

Correlated imaging is the process of imaging a specimen with two complementary modalities, and then combining the two data sets to create a highly informative, composite view. A recent implementation of this concept has been the combination of soft x-ray tomography (SXT) with fluorescence cryogenic microscopy (FCM). SXT-FCM is used to visualize cells that are held in a near-native, cryo-preserved state. The resultant images are, therefore, highly representative of both the cellular architecture and molecular organization in vivo. SXT quantitatively visualizes the cell and sub-cellular structures; FCM images the spatial distribution of fluorescently labeled molecules. Here, we review the characteristics of SXT-FCM, and briefly discuss how this method compares with existing correlative imaging techniques. We also describe how the incorporation of a cryo-rotation stage into a cryogenic fluorescence microscope allows acquisition of fluorescence cryogenic tomography (FCT) data. FCT is optimally suited to correlation with SXT, since both techniques image the specimen in 3-D, potentially with similar, isotropic spatial resolution. PMID:24355261

The feasibility study on 3-dimensional fluorescent x-ray computed tomography using the pinhole effect for biomedical applications.

PubMed

Sunaguchi, Naoki; Yuasa, Tetsuya; Hyodo, Kazuyuki; Zeniya, Tsutomu

2013-01-01

We propose a 3-dimensional fluorescent x-ray computed tomography (CT) pinhole collimator, aimed at providing molecular imaging with quantifiable measures and sub-millimeter spatial resolution. In this study, we demonstrate the feasibility of this concept and investigate imaging properties such as spatial resolution, contrast resolution and quantifiable measures, by imaging physical phantoms using a preliminary imaging system developed with monochromatic synchrotron x rays constructed at the BLNE-7A experimental line at KEK, Japan.

X-ray standing wave analysis of nanostructures using partially coherent radiation

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

Tiwari, M. K., E-mail: mktiwari@rrcat.gov.in; Das, Gangadhar; Bedzyk, M. J.

2015-09-07

The effect of longitudinal (or temporal) coherence on total reflection assisted x-ray standing wave (TR-XSW) analysis of nanoscale materials is quantitatively demonstrated by showing how the XSW fringe visibility can be strongly damped by decreasing the spectral resolution of the incident x-ray beam. The correction for nonzero wavelength dispersion (δλ ≠ 0) of the incident x-ray wave field is accounted for in the model computations of TR-XSW assisted angle dependent fluorescence yields of the nanostructure coatings on x-ray mirror surfaces. Given examples include 90 nm diameter Au nanospheres deposited on a Si(100) surface and a 3 nm thick Zn layer trapped on top amore » 100 nm Langmuir-Blodgett film coating on a Au mirror surface. Present method opens up important applications, such as enabling XSW studies of large dimensioned nanostructures using conventional laboratory based partially coherent x-ray sources.« less

Mitigation strategies against radiation-induced background for space astronomy missions

NASA Astrophysics Data System (ADS)

Davis, C. S. W.; Hall, D.; Keelan, J.; O'Farrell, J.; Leese, M.; Holland, A.

2018-01-01

The Advanced Telescope for High ENergy Astrophysics (ATHENA) mission is a major upcoming space-based X-ray observatory due to be launched in 2028 by ESA, with the purpose of mapping the early universe and observing black holes. Background radiation is expected to constitute a large fraction of the total system noise in the Wide Field Imager (WFI) instrument on ATHENA, and designing an effective system to reduce the background radiation impacting the WFI will be crucial for maximising its sensitivity. Significant background sources are expected to include high energy protons, X-ray fluorescence lines, 'knock-on' electrons and Compton electrons. Due to the variety of the different background sources, multiple shielding methods may be required to achieve maximum sensitivity in the WFI. These techniques may also be of great interest for use in future space-based X-ray experiments. Simulations have been developed to model the effect of a graded-Z shield on the X-ray fluorescence background. In addition the effect of a 90nm optical blocking filter on the secondary electron background has been investigated and shown to modify the requirements of any secondary electron shielding that is to be used.

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.

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.

Local atomic structure of Fe/Cr multilayers: Depth-resolved method

NASA Astrophysics Data System (ADS)

Babanov, Yu. A.; Ponomarev, D. A.; Devyaterikov, D. I.; Salamatov, Yu. A.; Romashev, L. N.; Ustinov, V. V.; Vasin, V. V.; Ageev, A. L.

2017-10-01

A depth-resolved method for the investigation of the local atomic structure by combining data of X-ray reflectivity and angle-resolved EXAFS is proposed. The solution of the problem can be divided into three stages: 1) determination of the element concentration profile with the depth z from X-ray reflectivity data, 2) determination of the X-ray fluorescence emission spectrum of the element i absorption coefficient μia (z,E) as a function of depth and photon energy E using the angle-resolved EXAFS data Iif (E , ϑl) , 3) determination of partial correlation functions gij (z , r) as a function of depth from μi (z , E) . All stages of the proposed method are demonstrated on a model example of a multilayer nanoheterostructure Cr/Fe/Cr/Al2O3. Three partial pair correlation functions are obtained. A modified Levenberg-Marquardt algorithm and a regularization method are applied.

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.

1998 Technology Showcase. JOAP International Condition Monitoring Conference.

DTIC Science & Technology

1998-04-01

Systems using Automated SEM/ EDX and New Diagnostic Routines 276 N. W Farrant & T. Luckhurst ADVANCED DIAGNOSTIC SYSTEMS Model-Based Diagnostics of Gas...Microscopy with Energy Dispersive X-Ray (SEM/ EDX ) micro analysis packages and Energy Dispersive X-Ray Fluorescence (EDXRF) analytical equipment. Therqfore...wear particles separated by ferrogram method. a- I WEAR PARTICLE A SLAS 97 (HOME PAGE) Fig I Home Page NONFE;RROUS MATERIAL A wW~ a48 -1, rV fr , ý b

3-D Cellular Ultrastructure Can Be Resolved by X-ray Microscopy | Center for Cancer Research

Cancer.gov

X-ray microscopy (XRM) is more rapid than cryoelectron tomography or super-resolution fluorescence microscopy and could fill an important gap in current technologies used to investigate in situ three-dimensional structure of cells. New XRM methods developed by first author Gerd Schneider, Ph.D., working with James McNally. Ph.D., and a team of colleagues, is capable of revealing full cellular ultrastructure without requiring fixation, staining, or sectioning.

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

Mazuritskiy, M. I., E-mail: mazurmik@gmail.com; Lerer, A. M.; Makhno, P. V.

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

Synchrotron applications in wood preservation and deterioration

Treesearch

Barbara L. Illman

2003-01-01

Several non-intrusive synchrotron techniques are being used to detect and study wood decay. The techniques use high intensity synchrotron-generated X-rays to determine the atomic structure of materials with imaging, diffraction, and absorption. Some of the techniques are X-ray absorption near edge structure (XANES), X-ray fluorescence spectroscopy (XFS), X-ray...

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

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 nanoprobes and diffraction-limited storage rings: opportunities and challenges of fluorescence tomography of biological specimens

PubMed Central

de Jonge, Martin D.; Ryan, Christopher G.; Jacobsen, Chris J.

2014-01-01

X-ray nanoprobes require coherent illumination to achieve optic-limited resolution, and so will benefit directly from diffraction-limited storage rings. Here, the example of high-resolution X-ray fluorescence tomography is focused on as one of the most voracious demanders of coherent photons, since the detected signal is only a small fraction of the incident flux. Alternative schemes are considered for beam delivery, sample scanning and detectors. One must consider as well the steps before and after the X-ray experiment: sample preparation and examination conditions, and analysis complexity due to minimum dose requirements and self-absorption. By understanding the requirements and opportunities for nanoscale fluorescence tomography, one gains insight into the R&D challenges in optics and instrumentation needed to fully exploit the source advances that diffraction-limited storage rings offer. PMID:25177992

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.

L X-ray fluorescence cross sections of some rare earth elements ( Z = 62, 64, 66, 68 and 70) at 17.8, 22.6 and 25.8 keV

NASA Astrophysics Data System (ADS)

Mandal, A. C.; Santra, S.; Mitra, D.; Sarkar, M.; Bhattacharya, D.

2005-06-01

L X-ray fluorescence cross sections of the elements with Z = 62, 64, 66, 68 and 70 have been measured at 17.8, 22.6 and 25.8 keV using an X-ray tube and secondary exciters of Mo, Ag and Sn. The measured cross sections have been compared with the theoretical predictions and with the data of others. Theoretical values calculated using photoionisation cross sections from Scofield [Lawrence Livermore Laboratory, UCRL-51326, 1973], fluorescence yields and Coster-Kronig transition probabilities from Puri et al. [X-ray Spectrom. 22 (1993) 358] and radiative widths from Campbell and Wang [At. Data Nucl. Data Tables 43 (1989) 281] show good agreement with our data. Except two sets of data on Lγ cross sections, all the data of other groups agree well with those of ours.

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

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

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 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.

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.

Determination of natural line widths of Kα X-ray lines for some elements in the atomic range 50≤Z≤65 at 59.5 keV

NASA Astrophysics Data System (ADS)

Kündeyi, Kadriye; Aylıkcı, Nuray Küp; Tıraşoǧlu, Engin; Kahoul, Abdelhalim; Aylıkcı, Volkan

2017-02-01

The semi-empirical determination of natural widths of Kα X-ray lines (Kα1 and Kα2) were performed for Sn, Sb, Te, I, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd and Tb. For the semi-empirical determination of the line widths, K shell fluorescence yields of elements were measured. The samples were excited by 59.5 keV γ rays from a 241Am annular radioactive source in order to measure the K shell fluorescence yields. The emitted K X-rays from the samples were counted by an Ultra-LEGe detector with a resolution of 150 eV at 5.9 keV. The measured K shell fluorescence yields were used for the calculation of K shell level widths. Finally, the natural widths of K X-ray lines were determined as the sums of levels which involved in the transition. The obtained values were compared with earlier studies.

40 CFR 80.46 - Measurement of reformulated gasoline and conventional gasoline fuel parameters.

Code of Federal Regulations, 2014 CFR

2014-07-01

... D7039-13, Standard Test Method for Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol Blends by Monochromatic Wavelength Dispersive X-ray Fluorescence...

Application of relativistic electrons for the quantitative analysis of trace elements

NASA Astrophysics Data System (ADS)

Hoffmann, D. H. H.; Brendel, C.; Genz, H.; Löw, W.; Richter, A.

1984-04-01

Particle induced X-ray emission methods (PIXE) have been extended to relativistic electrons to induce X-ray emission (REIXE) for quantitative trace-element analysis. The electron beam (20 ≤ E0≤ 70 MeV) was supplied by the Darmstadt electron linear accelerator DALINAC. Systematic measurements of absolute K-, L- and M-shell ionization cross sections revealed a scaling behaviour of inner-shell ionization cross sections from which X-ray production cross sections can be deduced for any element of interest for a quantitative sample investigation. Using a multielemental mineral monazite sample from Malaysia the sensitivity of REIXE is compared to well established methods of trace-element analysis like proton- and X-ray-induced X-ray fluorescence analysis. The achievable detection limit for very heavy elements amounts to about 100 ppm for the REIXE method. As an example of an application the investigation of a sample prepared from manganese nodules — picked up from the Pacific deep sea — is discussed, which showed the expected high mineral content of Fe, Ni, Cu and Ti, although the search for aliquots of Pt did not show any measurable content within an upper limit of 250 ppm.

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 are coded-aperture imagers, which have flown on ART-P, Integral, and Swift. The shadow pattern from a 50% full mask allows the distribution of X-rays from a wide (10s of degrees) field of view to be imaged, but uniform emission presents difficulties. A version of a coded-aperture plus CCD detector for airless bodies study is being built for OSIRIS-REx as the student experiment REXIS. We will show the quality of the spectra that can be expected from this class of instrument.

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).

High-temperature oxidation of advanced FeCrNi alloy in steam environments

DOE PAGES

Elbakhshwan, Mohamed S.; Gill, Simerjeet K.; Rumaiz, Abdul K.; ...

2017-07-04

Alloys of iron-chromium-nickel are being explored as alternative cladding materials to improve safety margins under severe accident conditions. Here, our research focuses on non-destructively investigating the oxidation behavior of the FeCrNi alloy “Alloy 33” using synchrotron-based methods. The evolution and structure of oxide layer formed in steam environments were characterized using X-ray diffraction, hard X-ray photoelectron spectroscopy, X-ray fluorescence methods and scanning electron microscopy. In conclusion, our results demonstrate that a compact and continuous oxide scale was formed consisting of two layers, chromium oxide and spinel phase (FeCr 2O 4) oxides, wherein the concentration of the FeCr 2O 4 phasemore » decreased from the surface to the bulk-oxide interface.« less

L-Cysteine capped CdTe-CdS core-shell quantum dots: preparation, characterization and immuno-labeling of HeLa cells.

PubMed

Zhang, Hongyan; Sun, Pan; Liu, Chang; Gao, Huanyu; Xu, Linru; Fang, Jin; Wang, Meng; Liu, Jinling; Xu, Shukun

2011-01-01

Functionalized CdTe-CdS core-shell quantum dots (QDs) were synthesized in aqueous solution via water-bathing combined hydrothermal method using L-cysteine (L-Cys) as a stabilizer. This method possesses both the advantages of water-bathing and hydrothermal methods for preparing high-quality QDs with markedly reduced synthesis time, and better stability than a lone hydrothermal method. The QDs were characterized by transmission electronic microscopy and powder X-ray diffraction and X-ray photoelectron spectroscopy. The CdTe-CdS QDs with core-shell structure showed both enhanced fluorescence and better photo stability than nude CdTe QDs. After conjugating with antibody rabbit anti-CEACAM8 (CD67), the as-prepared l-Cys capped CdTe-CdS QDs were successfully used as fluorescent probes for the direct immuno-labeling and imaging of HeLa cells. It was indicated that this kind of QD would have application potential in bio-labeling and cell imaging. Copyright © 2009 John Wiley & Sons, Ltd.

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

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

Ingerle, D.; Schiebl, M.; Streli, C.

2014-08-15

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

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

PubMed

Wang, Zhi-gang; Yu, Hong-mei

2012-01-01

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

Synthesis of a 3D lanthanum(III) MOFs as a multi-chemosensor to Cr(VI)-containing anion and Fe(III) cation based on a flexible ligand

NASA Astrophysics Data System (ADS)

Ma, Yang-Min; Liu, Tong; Huang, Wen-Huan

2018-02-01

Based on La(NO3)3·6H2O and 4,4‧-((5-carboxy-1,3-phenylene)bis(oxy))dibenzoic acid (H3cpbda), a 3D porous MOFs, [La(cpbda)(H2O)1.5]n (1), was synthesized by hydrothermal method and further characterized by single-crystal X-ray diffraction, power X-ray diffraction, IR spectroscopy, thermal-gravimetric analysis and fluorescence spectroscopy. Owing to its good stabilities and fluorescence property, the sensing experiments on sixteen cations and eleven anions were implemented. Moreover, the further titration processes show 1 can sensitively detect the Fe(III) cation and Cr(VI)-containing anions by quenching responses.

Iodine imaging in thyroid by fluorescent X-ray CT with 0.05 mm spatial resolution

NASA Astrophysics Data System (ADS)

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

2001-07-01

Fluorescent X-ray computed tomography (FXCT) at a 0.05 mm in-plane spatial resolution and 0.05 mm slice thickness depicted the cross sectional distribution of endogenous iodine within thyroid. The distribution obtained from the FXCT image correlated closely to that obtained from the pathological pictures.

A comparison between EGS4 and MCNP computer modeling of an in vivo X-ray fluorescence system.

PubMed

Al-Ghorabie, F H; Natto, S S; Al-Lyhiani, S H

2001-03-01

The Monte Carlo computer codes EGS4 and MCNP were used to develop a theoretical model of a 180 degrees geometry in vivo X-ray fluorescence system for the measurement of platinum concentration in head and neck tumors. The model included specification of the photon source, collimators, phantoms and detector. Theoretical results were compared and evaluated against X-ray fluorescence data obtained experimentally from an existing system developed by the Swansea In Vivo Analysis and Cancer Research Group. The EGS4 results agreed well with the MCNP results. However, agreement between the measured spectral shape obtained using the experimental X-ray fluorescence system and the simulated spectral shape obtained using the two Monte Carlo codes was relatively poor. The main reason for the disagreement between the results arises from the basic assumptions which the two codes used in their calculations. Both codes assume a "free" electron model for Compton interactions. This assumption will underestimate the results and invalidates any predicted and experimental spectra when compared with each other.

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

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

Choudhury, Sanjukta; Thomas, Jith; Sylvain, Nicole J.

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

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

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

Worley, C. G.; Wiltshire, S.; Miller, T. C.

A method was developed to detect fingerprints using a technique known as micro-X-ray fluorescence. The traditional method of detecting fingerprints involves treating the sample with certain powders, liquids, or vapors to add color to the fingerprint so that it can be easily seen and photographed for forensic purposes. This is known as contrast enhancement, and a multitude of chemical processing methods have been developed in the past century to render fingerprints visible. However, fingerprints present on certain substances such as fibrous papers and textiles, wood, leather, plastic, adhesives, and human skin can sometimes be difficult to detect by contrast enhancement.more » Children's fingerprints are also difficult to detect due to the absence of sebum on their skin, and detection of prints left on certain colored backgrounds can sometimes be problematic. Micro-X-ray fluorescence (MXRF) was studied here as a method to detect fingerprints based on chemical elements present in fingerprint residue. For example, salts such as sodium chloride and potassium chloride excreted in sweat are sometimes present in detectable quantities in fingerprints. We demonstrated that MXRF can be used to detect this sodium, potassium, and chlorine from such salts. Furthermore, using MXRF, each of these elements (and many other elements if present) can be detected as a function of location on a surface, so we were able to 'see' a fingerprint because these salts are deposited mainly along the patterns present in a fingerprint (traditionally called friction ridges in forensic science). MXRF is not a panacea for detecting all fingerprints; some prints will not contain enough detectable material to be 'seen'; however, determining an effective means of coloring a fingerprint with traditional contrast enhancement methods can sometimes be an arduous process with limited success. Thus, MXRF offers a possible alternative for detecting fingerprints, and it does not require any additional chemical treatment steps which can be time consuming and permanently alter the sample. Additionally, MXRF is noninvasive, so a fingerprint analyzed by this method is left pristine for examination by other methods (eg. DNA extraction). To the best of the author's knowledge, no studies have been published to date concerning the detection of fingerprints by micro-X-ray fluorescence. Some studies have been published in which other spectroscopic methods were employed to examine the chemical composition of fingerprints (eg. IR, SEM/EDX, and Auger), but very few papers discuss the actual detection and imaging of a complete fingerprint by any spectroscopic method. Thus, this work is unique.« less

Determination of K shell absorption jump factors and jump ratios of 3d transition metals by measuring K shell fluorescence parameters.

PubMed

Kaçal, Mustafa Recep; Han, İbrahim; Akman, Ferdi

2015-01-01

Energy dispersive X-ray fluorescence technique (EDXRF) has been employed for measuring K-shell absorption jump factors and jump ratios for Ti, Cr, Fe, Co, Ni and Cu elements. The jump factors and jump ratios for these elements were determined by measuring K shell fluorescence parameters such as the Kα X-ray production cross-sections, K shell fluorescence yields, Kβ-to-Kα X-rays intensity ratios, total atomic absorption cross sections and mass attenuation coefficients. The measurements were performed using a Cd-109 radioactive point source and an Si(Li) detector in direct excitation and transmission experimental geometry. The measured values for jump factors and jump ratios were compared with theoretically calculated and the ones available in the literature. Copyright © 2014 Elsevier Ltd. All rights reserved.

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.

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.

40 CFR Appendix A to Subpart Uuu... - Determination of Metal Concentration on Catalyst Particles (Instrumental Analyzer Procedure)

Code of Federal Regulations, 2010 CFR

2010-07-01

... either energy or wavelength dispersive X-ray flourescent (XRF) spectrometry instrumental analyzers. In both types of XRF spectrometers, the instrument irradiates the sample with high energy (primary) x-rays and the elements in the sample absorb the x-rays and then re-emit secondary (fluorescent) x-rays of...

40 CFR Appendix A to Subpart Uuu... - Determination of Metal Concentration on Catalyst Particles (Instrumental Analyzer Procedure)

Code of Federal Regulations, 2011 CFR

2011-07-01

... either energy or wavelength dispersive X-ray flourescent (XRF) spectrometry instrumental analyzers. In both types of XRF spectrometers, the instrument irradiates the sample with high energy (primary) x-rays and the elements in the sample absorb the x-rays and then re-emit secondary (fluorescent) x-rays of...

Determination of selenium at trace levels in geologic materials by energy-dispersive X-ray fluorescence spectrometry

USGS Publications Warehouse

Wahlberg, J.S.

1981-01-01

Low levels of selenium (0.1-500 ppm) in both organic and inorganic geologic materials can be semiquantitatively measured by isolating Se as a thin film for presentation to an energy-dispersive X-ray fluorescence spectrometer. Suitably pulverized samples are first digested by fusing with a mixture of Na2CO3 and Na2O2. The fusion cake is dissolved in distilled water, buffered with NH4Cl, and filtered to remove Si and the R2O3 group. A carrier solution of Na2TeO4, plus solid KI, hydrazine sulfate and Na2SO3, is added to the filtrate. The solution is then vacuum-filtered through a 0.45-??m pore-size filter disc. The filter, with the thin film of precipitate, is supported between two sheets of Mylar?? film for analysis. Good agreement is shown between data reported in this study and literature values reported by epithermal neutron-activation analysis and spectrofluorimetry. The method can be made quantitative by utilizing a secondary precipitation to assure complete recovery of the Se. The X-ray method offers fast turn-around time and a reasonably high production rate. ?? 1981.

Waiting in the Wings: Reflected X-ray Emission from the Homunculus Nebula

NASA Technical Reports Server (NTRS)

Corcoran, M. F.; Hamaguchi, K.; Gull, T.; Davidson, K.; Petre, R.; Hillier, D. J.; Smith, N.; Damineli, A.; Morse, J. A.; Walborn, N. R.

2004-01-01

We report the first detection of X-ray emission associated with the Homunculus Nebula which surrounds the supermassive star eta Carinae. The emission is characterized by a temperature in excess of 100 MK, and is consistent with scattering of the time-delayed X-ray flux associated with the star. The nebular emission is bright in the northwestern lobe and near the central regions of the Homunculus, and fainter in the southeastern lobe. We also report the detection of an unusually broad Fe K fluorescent line, which may indicate fluorescent scattering off the wind of a companion star or some other high velocity outflow. The X-ray Homunculus is the nearest member of the small class of Galactic X-ray reflection nebulae, and the only one in which both the emitting and reflecting sources are distinguishable.

Influence of reaction time and synthesis temperature on the physical properties of ZnO nanoparticles synthesized by the hydrothermal method

NASA Astrophysics Data System (ADS)

Wasly, H. S.; El-Sadek, M. S. Abd; Henini, Mohamed

2018-01-01

Influence of synthesis temperature and reaction time on the structural and optical properties of ZnO nanoparticles synthesized by the hydrothermal method was investigated using X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), energy-dispersive X-ray, Fourier transform infra-red spectroscopy, and UV-visible and fluorescence spectroscopy. The XRD pattern and HR-TEM images confirmed the presence of crystalline hexagonal wurtzite ZnO nanoparticles with average crystallite size in the range 30-40 nm. Their energy gap determined by fluorescence was found to depend on the synthesis temperature and reaction time with values in the range 2.90-3.78 eV. Thermal analysis, thermogravimetric and the differential scanning calorimetry were used to study the thermal reactions and weight loss with heat of the prepared ZnO nanoparticles.

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

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

Tellería Narvaez, C.A.; Fernández Alcázar, S.; Barrientos Zamora, F.G.

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

Beam position monitor

DOEpatents

Alkire, Randy W.; Rosenbaum, Gerold; Evans, Gwyndaf

2003-07-22

An apparatus for determining the position of an x-ray beam relative to a desired beam axis. Where the apparatus is positioned along the beam path so that a thin metal foil target intersects the x-ray beam generating fluorescent radiation. A PIN diode array is positioned so that a portion of the fluorescent radiation is intercepted by the array resulting in an a series of electrical signals from the PIN diodes making up the array. The signals are then analyzed and the position of the x-ray beam is determined relative to the desired beam path.

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

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

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.

Quantitative imaging of gold nanoparticle distribution in a tumor-bearing mouse using benchtop x-ray fluorescence computed tomography

PubMed Central

Manohar, Nivedh; Reynoso, Francisco J.; Diagaradjane, Parmeswaran; Krishnan, Sunil; Cho, Sang Hyun

2016-01-01

X-ray fluorescence computed tomography (XFCT) is a technique that can identify, quantify, and locate elements within objects by detecting x-ray fluorescence (characteristic x-rays) stimulated by an excitation source, typically derived from a synchrotron. However, the use of a synchrotron limits practicality and accessibility of XFCT for routine biomedical imaging applications. Therefore, we have developed the ability to perform XFCT on a benchtop setting with ordinary polychromatic x-ray sources. Here, we report our postmortem study that demonstrates the use of benchtop XFCT to accurately image the distribution of gold nanoparticles (GNPs) injected into a tumor-bearing mouse. The distribution of GNPs as determined by benchtop XFCT was validated using inductively coupled plasma mass spectrometry. This investigation shows drastically enhanced sensitivity and specificity of GNP detection and quantification with benchtop XFCT, up to two orders of magnitude better than conventional x-ray CT. The results also reaffirm the unique capabilities of benchtop XFCT for simultaneous determination of the spatial distribution and concentration of nonradioactive metallic probes, such as GNPs, within the context of small animal imaging. Overall, this investigation identifies a clear path toward in vivo molecular imaging using benchtop XFCT techniques in conjunction with GNPs and other metallic probes. PMID:26912068

Analysis of coke beverages by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; von Bohlen, Alex; Friedrich K, E. Josue; Redrejo, M. J.

2018-07-01

The influence of the organic content, sample preparation process and the morphology of the depositions of two types of Coke beverage, traditional and light Coke, have been investigated by mean of Total-reflection X-ray Fluorescence (TXRF) spectrometry. Strong distortions of the nominal concentration values, up to 128% for P, have been detected in the analysis of traditional Coke by different preparation methods. These differences have been correlated with the edge X-ray energies of the elements analyzed being more pronounced for the lighter elements. The influence of the organic content (mainly sugar) was evaluated comparing traditional and light Coke analytical TXRF results. Three sample preparation methods have been evaluated as follows: direct TXRF analysis of the sample only adding internal standard, TXRF analysis after open vessel acid digestion and TXRF analysis after high pressure and temperature microwave-assisted acid digestion. Strong correlations were detected between quantitative results, methods of preparation and energies of the X-ray absorption edges of quantified elements. In this way, a decay behavior for the concentration differences between preparation methods and the energies of the X-ray absorption edges of each element were observed. The observed behaviors were modeled with exponential decay functions obtaining R2 correlation coefficients from 0.989 to 0.992. The strong absorption effect observed, and even possible matrix effect, can be explained by the inherent high organic content of the evaluated samples and also by the morphology and average thickness of the TXRF depositions observed. As main conclusion of this work, the analysis of light elements in samples with high organic content by TXRF, i.e. medical, biological, food or any other organic matrixes should be taken carefully. In any case, the direct analysis is not recommended and a previous microwave-assisted acid digestion, or similar, is mandatory, for the correct elemental quantification by TXRF.

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 reconstruction showed that for a scatter magnitude decrease by a factor of 2.4, the molecular sensitivity could almost be doubled. Scatter reduction lowers the amount of noise in the projection datasets and reconstructed images which enhance molecular sensitivity at equal dose. The results support the use of linear polarized x rays to reduce scatter in XFCT imaging. © 2018 American Association of Physicists in Medicine.

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.…

Publications - GMC 264 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 264 Publication Details Title: X-ray fluorescence trace element data of the following U.S for more information. Bibliographic Reference Werdon, M.B., 1996, X-ray fluorescence trace element . Bureau of Mines hard rock mineral pulp samples from the Colville mining district: West Kivliktort

Palus Somni - Anomalies in the correlation of Al/Si X-ray fluorescence intensity ratios and broad-spectrum visible albedos. [lunar surface mineralogy

NASA Technical Reports Server (NTRS)

Clark, P. E.; Andre, C. G.; Adler, I.; Weidner, J.; Podwysocki, M.

1976-01-01

The positive correlation between Al/Si X-ray fluorescence intensity ratios determined during the Apollo 15 lunar mission and a broad-spectrum visible albedo of the moon is quantitatively established. Linear regression analysis performed on 246 1 degree geographic cells of X-ray fluorescence intensity and visible albedo data points produced a statistically significant correlation coefficient of .78. Three distinct distributions of data were identified as (1) within one standard deviation of the regression line, (2) greater than one standard deviation below the line, and (3) greater than one standard deviation above the line. The latter two distributions of data were found to occupy distinct geographic areas in the Palus Somni region.

Performance dependence of hybrid x-ray computed tomography/fluorescence molecular tomography on the optical forward problem.

PubMed

Hyde, Damon; Schulz, Ralf; Brooks, Dana; Miller, Eric; Ntziachristos, Vasilis

2009-04-01

Hybrid imaging systems combining x-ray computed tomography (CT) and fluorescence tomography can improve fluorescence imaging performance by incorporating anatomical x-ray CT information into the optical inversion problem. While the use of image priors has been investigated in the past, little is known about the optimal use of forward photon propagation models in hybrid optical systems. In this paper, we explore the impact on reconstruction accuracy of the use of propagation models of varying complexity, specifically in the context of these hybrid imaging systems where significant structural information is known a priori. Our results demonstrate that the use of generically known parameters provides near optimal performance, even when parameter mismatch remains.

Argon content of the Martian atmosphere at the Viking 1 landing site - Analysis by X-ray fluorescence spectroscopy

NASA Technical Reports Server (NTRS)

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

1976-01-01

Spectra provided by the Viking 1 X-ray fluorescence spectrometer operating in the calibration mode (without a soil sample in the analysis chamber) were analyzed to determine the argon content of the Martian atmosphere at the landing site. This was found to be less than or equal to 0.15 millibar, or not more than 2% by volume, consistent with data obtained by the entry mass spectrometer and by the mass spectrometer on the lander. It is anticipated that analysis of the K content of surface samples using X-ray fluorescence data will provide information on the evolution of the atmosphere, since most atmospheric argon is apparently produced by decay of K-40.

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.

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

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.

The fundamental parameter method applied to X-ray fluorescence analysis with synchrotron radiation

NASA Astrophysics Data System (ADS)

Pantenburg, F. J.; Beier, T.; Hennrich, F.; Mommsen, H.

1992-05-01

Quantitative X-ray fluorescence analysis applying the fundamental parameter method is usually restricted to monochromatic excitation sources. It is shown here, that such analyses can be performed as well with a white synchrotron radiation spectrum. To determine absolute elemental concentration values it is necessary to know the spectral distribution of this spectrum. A newly designed and tested experimental setup, which uses the synchrotron radiation emitted from electrons in a bending magnet of ELSA (electron stretcher accelerator of the university of Bonn) is presented. The determination of the exciting spectrum, described by the given electron beam parameters, is limited due to uncertainties in the vertical electron beam size and divergence. We describe a method which allows us to determine the relative and absolute spectral distributions needed for accurate analysis. First test measurements of different alloys and standards of known composition demonstrate that it is possible to determine exact concentration values in bulk and trace element analysis.

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

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.

Evaluation of the dose received in the tissues of the neck during quantification of iodine in the thyroid by X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Portararo, Antonio; Licour, Caroline; Gerardy, Isabelle; Pozuelo Navarro, Fausto

2018-04-01

The determination of the iodine content in the thyroid is of great interest for many investigations of this gland. The conventional scintigraphic method, using radionuclides, is efficient but delivers a significant dose to the patient. The X-ray fluorescence spectrometry could give information about the iodine content in the thyroid. The measured signal is obtained after stimulation of the stable iodine contained in the gland by X-rays. The advantage of this technique is the complete absence of radioactive isotope injected into the patient body. By applying this, a decrease in effective dose to the patient should be obtained. In this work, the study of the dose received by a thyroid phantom (surrounded by the different tissues of the neck) was performed. The phantom is made of PLA. The dose is measured in optimised conditions defined for the analytical technique. A total head-neck phantom was also used in order to consider the absorbed dose in each different tissues and organs as spinal cord or eyes. Thermo-luminescence dosimeters were chosen for their small size, their sensitivity and the easy positioning on the surface of the phantom but also inside of it to evaluate dose to internal organs. Those LiF 100 dosimeters have been calibrated within the X-ray beam also used for the analysis of iodine. The repeatability and reproducibility of the method has been evaluated. The influence of parameters as concentration of iodine in the thyroid, distance between the X-ray generator and the neck, thickness of the tissues surrounding the thyroid, has been investigated in terms of modifying parameters of the dose received by different tissues situated in the neck and the head.

Preserving elemental content in adherent mammalian cells for analysis by synchrotron-based x-ray fluorescence microscopy

DOE PAGES

Jin, Qiaoling; Paunesku, Tatjana; Lai, Barry; ...

2016-08-31

Trace metals play important roles in biological function, and x-ray fluorescence microscopy (XFM) provides a way to quantitatively image their distribution within cells. The faithfulness of these measurements is dependent on proper sample preparation. Using mouse embryonic fibroblast NIH/3T3 cells as an example, we compare various approaches to the preparation of adherent mammalian cells for XFM imaging under ambient temperature. Direct side-by-side comparison shows that plunge-freezing-based cryoimmobilization provides more faithful preservation than conventional chemical fixation for most biologically important elements including P, S, Cl, K, Fe, Cu, Zn and possibly Ca in adherent mammalian cells. Although cells rinsed with freshmore » media had a great deal of extracellular background signal for Cl and Ca, this approach maintained cells at the best possible physiological status before rapid freezing and it does not interfere with XFM analysis of other elements. If chemical fixation has to be chosen, the combination of 3% paraformaldehyde and 1.5 % glutaraldehyde preserves S, Fe, Cu and Zn better than either fixative alone. Lastly, when chemically fixed cells were subjected to a variety of dehydration processes, air drying was proved to be more suitable than other drying methods such as graded ethanol dehydration and freeze drying. This first detailed comparison for x-ray fluorescence microscopy shows how detailed quantitative conclusions can be affected by the choice of cell preparation method.« less

Preserving elemental content in adherent mammalian cells for analysis by synchrotron-based x-ray fluorescence microscopy

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

Jin, Qiaoling; Paunesku, Tatjana; Lai, Barry

Trace metals play important roles in biological function, and x-ray fluorescence microscopy (XFM) provides a way to quantitatively image their distribution within cells. The faithfulness of these measurements is dependent on proper sample preparation. Using mouse embryonic fibroblast NIH/3T3 cells as an example, we compare various approaches to the preparation of adherent mammalian cells for XFM imaging under ambient temperature. Direct side-by-side comparison shows that plunge-freezing-based cryoimmobilization provides more faithful preservation than conventional chemical fixation for most biologically important elements including P, S, Cl, K, Fe, Cu, Zn and possibly Ca in adherent mammalian cells. Although cells rinsed with freshmore » media had a great deal of extracellular background signal for Cl and Ca, this approach maintained cells at the best possible physiological status before rapid freezing and it does not interfere with XFM analysis of other elements. If chemical fixation has to be chosen, the combination of 3% paraformaldehyde and 1.5 % glutaraldehyde preserves S, Fe, Cu and Zn better than either fixative alone. Lastly, when chemically fixed cells were subjected to a variety of dehydration processes, air drying was proved to be more suitable than other drying methods such as graded ethanol dehydration and freeze drying. This first detailed comparison for x-ray fluorescence microscopy shows how detailed quantitative conclusions can be affected by the choice of cell preparation method.« less

Method And Apparatus For Detecting Chemical Binding

DOEpatents

Warner, Benjamin P.; Havrilla, George J.; Miller, Thomasin C.; Wells, Cyndi A.

2005-02-22

The method for screening binding between a target binder and potential pharmaceutical chemicals involves sending a solution (preferably an aqueous solution) of the target binder through a conduit to a size exclusion filter, the target binder being too large to pass through the size exclusion filter, and then sending a solution of one or more potential pharmaceutical chemicals (preferably an aqueous solution) through the same conduit to the size exclusion filter after target binder has collected on the filter. The potential pharmaceutical chemicals are small enough to pass through the filter. Afterwards, x-rays are sent from an x-ray source to the size exclusion filter, and if the potential pharmaceutical chemicals form a complex with the target binder, the complex produces an x-ray fluorescence signal having an intensity that indicates that a complex has formed.

Method and apparatus for detecting chemical binding

DOEpatents

Warner, Benjamin P [Los Alamos, NM; Havrilla, George J [Los Alamos, NM; Miller, Thomasin C [Los Alamos, NM; Wells, Cyndi A [Los Alamos, NM

2007-07-10

The method for screening binding between a target binder and potential pharmaceutical chemicals involves sending a solution (preferably an aqueous solution) of the target binder through a conduit to a size exclusion filter, the target binder being too large to pass through the size exclusion filter, and then sending a solution of one or more potential pharmaceutical chemicals (preferably an aqueous solution) through the same conduit to the size exclusion filter after target binder has collected on the filter. The potential pharmaceutical chemicals are small enough to pass through the filter. Afterwards, x-rays are sent from an x-ray source to the size exclusion filter, and if the potential pharmaceutical chemicals form a complex with the target binder, the complex produces an x-ray fluorescence signal having an intensity that indicates that a complex has formed.

Normal incidence X-ray mirror for chemical microanalysis

DOEpatents

Carr, Martin J.; Romig, Jr., Alton D.

1990-01-01

A non-planar, focusing mirror, to be utilized in both electron column instruments and micro-x-ray fluorescence instruments for performing chemical microanalysis on a sample, comprises a concave, generally spherical base substrate and a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on the base substrate. The thickness of each layer is an integral multiple of the wavelength being reflected and may vary non-uniformly according to a predetermined design. The chemical analytical instruments in which the mirror is used also include a predetermined energy source for directing energy onto the sample and a detector for receiving and detecting the x-rays emitted from the sample; the non-planar mirror is located between the sample and detector and collects the x-rays emitted from the sample at a large solid angle and focuses the collected x-rays to the sample. For electron column instruments, the wavelengths of interest lie above 1.5 nm, while for x-ray fluorescence instruments, the range of interest is below 0.2 nm. Also, x-ray fluorescence instruments include an additional non-planar focusing mirror, formed in the same manner as the previously described m The invention described herein was made in the performance of work under contract with the Department of Energy, Contract No. DE-AC04-76DP00789, and the United States Government has rights in the invention pursuant to this contract.

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.

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

DTIC Science & Technology

2008-04-01

from magnesium (Mg) to uranium (U) using two X-ray detection sensors: a FOCUS 5+ detector AlX-ray tube X-ray Detector 1. Incident X-ray...zinc (Zn), whilst the PIN detector is used to detect elements from calcium (Ca) to uranium (U) [4]. Elements between calcium (Ca) to zinc (Zn) can be... carbide paper, however polishing is not a normal sample preparation requirement for the Twin-X (see Figure 16). The samples were placed polished side

Tracking ink composition on Herculaneum papyrus scrolls: quantification and speciation of lead by X-ray based techniques and Monte Carlo simulations.

PubMed

Tack, Pieter; Cotte, Marine; Bauters, Stephen; Brun, Emmanuel; Banerjee, Dipanjan; Bras, Wim; Ferrero, Claudio; Delattre, Daniel; Mocella, Vito; Vincze, Laszlo

2016-02-08

The writing in carbonized Herculaneum scrolls, covered and preserved by the pyroclastic events of the Vesuvius in 79 AD, was recently revealed using X-ray phase-contrast tomography, without the need of unrolling the sensitive scrolls. Unfortunately, some of the text is difficult to read due to the interference of the papyrus fibers crossing the written text vertically and horizontally. Recently, lead was found as an elemental constituent in the writing, rendering the text more clearly readable when monitoring the lead X-ray fluorescence signal. Here, several hypotheses are postulated for the origin and state of lead in the papyrus writing. Multi-scale X-ray fluorescence micro-imaging, Monte Carlo quantification and X-ray absorption microspectroscopy experiments are used to provide additional information on the ink composition, in an attempt to determine the origin of the lead in the Herculaneum scrolls and validate the postulated hypotheses.

Small Angle X-Ray Scattering Detector

DOEpatents

Hessler, Jan P.

2004-06-15

A detector for time-resolved small-angle x-ray scattering includes a nearly constant diameter, evacuated linear tube having an end plate detector with a first fluorescent screen and concentric rings of first fiber optic bundles for low angle scattering detection and an annular detector having a second fluorescent screen and second fiber optic bundles concentrically disposed about the tube for higher angle scattering detection. With the scattering source, i.e., the specimen under investigation, located outside of the evacuated tube on the tube's longitudinal axis, scattered x-rays are detected by the fiber optic bundles, to each of which is coupled a respective photodetector, to provide a measurement resolution, i.e., dq/q, where q is the momentum transferred from an incident x-ray to an x-ray scattering specimen, of 2% over two (2) orders of magnitude in reciprocal space, i.e., q.sub.max /q.sub.min.congruent.100.

Pressure mapping for sphere and half-sphere enhanced diamond anvil cells using synchrotron x-ray diffraction and fluorescence techniques

NASA Astrophysics Data System (ADS)

Liu, H.; Liu, L. L.; Cai, Z.; Shu, J.

2015-12-01

The measurement for equation of state (EoS) of materials under pressure conditions above 200 GPa is a long-standing challenging subject. Recently, second stage anvil, which was loaded inside the diamond anvil cell (DAC), had been reported by various groups. This method could generate pressure over 300 GPa, or above 600 GPa from the EoS measurement of Re metal between the tiny anvil or 2 half-spheres. Several alternative approaches, using ruby balls, or glassy carbon, or diamond, with single sphere, 2 half-spheres, or multi spheres geometry inside DAC, were tested. The NIST X-ray powder standard, ZnO was selected as pressure marker. Focused ion beam (FIB) was used to cut the half-sphere from diamond anvil top directly to avoid the difficulty of alignment. The synchrotron x-ray diffraction with fine beam size down to 100 nm using zone plate set-up was used to map the pressure gradient at the sphere or half-sphere zone inside DAC. The pressure could be boosted at center of sphere by up to 10 - 70 GPa at about 200 GPa conditions. From broken anvils, trace element analysis using fine focusing synchrotron x-ray fluorescence method revealed the potential anvil damage from FIB cutting the diamond anvil tip, which might decrease the strength of anvils. Fine touch from FIB cutting at final stage using low ion beam current is suggested.

Determination of trace metals in spirits by total reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Siviero, G.; Cinosi, A.; Monticelli, D.; Seralessandri, L.

2018-06-01

Eight spirituous samples were analyzed for trace metal content with Horizon Total Reflection X-Ray Fluorescence (TXRF) Spectrometer. The expected single metal amount is at the ng/g level in a mixed aqueous/organic matrix, thus requiring a sample preparation method capable of achieving suitable limits of detection. On-site enrichment and Atmospheric Pressure-Vapor Phase Decomposition allowed to detect Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sr and Pb with detection limits ranging from 0.1 ng/g to 4.6 ng/g. These results highlight how the synergy between instrument and sample preparation strategy may foster the use of TXRF as a fast and reliable technique for the determination of trace elements in spirituous samples, either for quality control or risk assessment purposes.

Element sensitive reconstruction of nanostructured surfaces with finite elements and grazing incidence soft X-ray fluorescence.

PubMed

Soltwisch, Victor; Hönicke, Philipp; Kayser, Yves; Eilbracht, Janis; Probst, Jürgen; Scholze, Frank; Beckhoff, Burkhard

2018-03-29

The geometry of a Si3N4 lamellar grating was investigated experimentally with reference-free grazing-incidence X-ray fluorescence analysis. While simple layered systems are usually treated with the matrix formalism to determine the X-ray standing-wave field, this approach fails for laterally structured surfaces. Maxwell solvers based on finite elements are often used to model electrical field strengths for any 2D or 3D structures in the optical spectral range. We show that this approach can also be applied in the field of X-rays. The electrical field distribution obtained with the Maxwell solver can subsequently be used to calculate the fluorescence intensities in full analogy to the X-ray standing-wave field obtained by the matrix formalism. Only the effective 1D integration for the layer system has to be replaced by a 2D integration of the finite elements, taking into account the local excitation conditions. We will show that this approach is capable of reconstructing the geometric line shape of a structured surface with high elemental sensitivity. This combination of GIXRF and finite-element simulations paves the way for a versatile characterization of nanoscale-structured surfaces.

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 environments will be presented.

Dendrochemical patterns of calcium, zinc, and potassium related to internal factors detected by energy dispersive X-ray fluorescence (EDXRF)

Treesearch

Kevin T. Smith; Jean Christophe Balouet; Walter C. Shortle; Michel Chalot; François Beaujard; Hakan Grudd; Don A. Vroblesky; Joel G. Burken

2014-01-01

Energy dispersive X-ray fluorescence (EDXRF) provides highly sensitive and precise spatial resolution of cation content in individual annual growth rings in trees. The sensitivity and precision have prompted successful applications to forensic dendrochemistry and the timing of environmental releases of contaminants. These applications have highlighted the need to...

Synchrotron-based X-ray Fluorescence Microscopy in Conjunction with Nanoindentation to Study Molecular-Scale Interactions of Phenol–Formaldehyde in Wood Cell Walls

Treesearch

Joseph E. Jakes; Christopher G. Hunt; Daniel J. Yelle; Linda Lorenz; Kolby Hirth; Sophie-Charlotte Gleber; Stefan Vogt; Warren Grigsby; Charles R. Frihart

2015-01-01

Understanding and controlling molecular-scale interactions between adhesives and wood polymers are critical to accelerate the development of improved adhesives for advanced wood-based materials. The submicrometer resolution of synchrotron-based X-ray fluorescence microscopy (XFM) was found capable of mapping and quantifying infiltration of Br-labeled phenol−...

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND ROUTINE USE OF THE SPECTRACE 9000 FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER (UA-L-10.1)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for operating and calibrating the Spectrace 9000 field portable X-ray fluorescence analyzer. This procedure applies to the determination of metal concentrations in samples during the Arizona NHEXAS project and the "Border" st...

The use of a multi-method approach to identify the pigments in the 12th century manuscript Liber Floridus

NASA Astrophysics Data System (ADS)

Deneckere, A.; De Reu, M.; Martens, M. P. J.; De Coene, K.; Vekemans, B.; Vincze, L.; De Maeyer, Ph.; Vandenabeele, P.; Moens, L.

2011-10-01

A selection of illuminations of the 12th century manuscript Liber Floridus was analysed with Raman spectroscopy (in situ and laboratory measurements), X-ray fluorescence spectroscopy, UV-fluorescence photography and infrared reflectography (IRR). The aim of this study is to determine the pigments used, in order to search for anachronisms. Using a combination of Raman spectroscopy (molecular information) and X-ray fluorescence spectroscopy (elemental information) following pigments could be identified: ultramarine (Na 8-10Al 6Si 6O 24S 2-4), azurite (2CuCO 3·Cu(OH) 2), caput mortuum (Fe 2O 3), vermilion (HgS), orpiment (As 2S 3) and lead white (2PbCO 3·Pb(OH) 2). Moreover, two synthetic red pigments, PR4 and PR176, and a degradation product, gypsum (CaSO 4·2H 2O), were present in the manuscript. To establish the origin of the modern materials UV-fluorescence photography was used. Infrared reflectography (IRR) was applied to visualise the underdrawing of the investigated folios.

Correlative cryogenic tomography of cells using light and soft x-rays.

PubMed

Smith, Elizabeth A; Cinquin, Bertrand P; Do, Myan; McDermott, Gerry; Le Gros, Mark A; Larabell, Carolyn A

2014-08-01

Correlated imaging is the process of imaging a specimen with two complementary modalities, and then combining the two data sets to create a highly informative, composite view. A recent implementation of this concept has been the combination of soft x-ray tomography (SXT) with fluorescence cryogenic microscopy (FCM). SXT-FCM is used to visualize cells that are held in a near-native, cryopreserved. The resultant images are, therefore, highly representative of both the cellular architecture and molecular organization in vivo. SXT quantitatively visualizes the cell and sub-cellular structures; FCM images the spatial distribution of fluorescently labeled molecules. Here, we review the characteristics of SXT-FCM, and briefly discuss how this method compares with existing correlative imaging techniques. We also describe how the incorporation of a cryo-rotation stage into a cryogenic fluorescence microscope allows acquisition of fluorescence cryogenic tomography (FCT) data. FCT is optimally suited for correlation with SXT, since both techniques image the specimen in 3-D, potentially with similar, isotropic spatial resolution. © 2013 Elsevier B.V. All rights reserved.

X ray sensitive area detection device

NASA Technical Reports Server (NTRS)

Carter, Daniel C. (Inventor); Witherow, William K. (Inventor); Pusey, Marc L. (Inventor); Yost, Vaughn H. (Inventor)

1990-01-01

A radiation sensitive area detection device is disclosed which comprises a phosphor-containing film capable of receiving and storing an image formed by a pattern of incoming x rays, UV, or other radiation falling on the film. The device is capable of fluorescing in response to stimulation by a light source in a manner directly proportional to the stored radiation pattern. The device includes: (1) a light source capable of projecting light or other appropriate electromagnetic wave on the film so as to cause it to fluoresce; (2) a means to focus the fluoresced light coming from the phosphor-containing film after light stimulation; and (3) at least one charged coupled detector or other detecting element capable of receiving and digitizing the pattern of fluoresced light coming from the phosphor-containing film. The device will be able to generate superior x ray images of high resolution from a crystal or other sample and will be particularly advantageous in that instantaneous near-real-time images of rapidly deteriorating samples can be obtained. Furthermore, the device can be made compact and sturdy, thus capable of carrying out x ray or other radiation imaging under a variety of conditions, including those experienced in space.

Hard-X-ray dark-field imaging using a grating interferometer.

PubMed

Pfeiffer, F; Bech, M; Bunk, O; Kraft, P; Eikenberry, E F; Brönnimann, Ch; Grünzweig, C; David, C

2008-02-01

Imaging with visible light today uses numerous contrast mechanisms, including bright- and dark-field contrast, phase-contrast schemes and confocal and fluorescence-based methods. X-ray imaging, on the other hand, has only recently seen the development of an analogous variety of contrast modalities. Although X-ray phase-contrast imaging could successfully be implemented at a relatively early stage with several techniques, dark-field imaging, or more generally scattering-based imaging, with hard X-rays and good signal-to-noise ratio, in practice still remains a challenging task even at highly brilliant synchrotron sources. In this letter, we report a new approach on the basis of a grating interferometer that can efficiently yield dark-field scatter images of high quality, even with conventional X-ray tube sources. Because the image contrast is formed through the mechanism of small-angle scattering, it provides complementary and otherwise inaccessible structural information about the specimen at the micrometre and submicrometre length scale. Our approach is fully compatible with conventional transmission radiography and a recently developed hard-X-ray phase-contrast imaging scheme. Applications to X-ray medical imaging, industrial non-destructive testing and security screening are discussed.

X-ray data booklet. Revision

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

Vaughan, D.

A compilation of data is presented. Included are properties of the elements, electron binding energies, characteristic x-ray energies, fluorescence yields for K and L shells, Auger energies, energy levels for hydrogen-, helium-, and neonlike ions, scattering factors and mass absorption coefficients, and transmission bands of selected filters. Also included are selected reprints on scattering processes, x-ray sources, optics, x-ray detectors, and synchrotron radiation facilities. (WRF)

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.

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.

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.

Measurements of K shell absorption jump factors and jump ratios using EDXRF technique

NASA Astrophysics Data System (ADS)

Kacal, Mustafa Recep; Han, İbrahim; Akman, Ferdi

2015-04-01

In the present work, the K-shell absorption jump factors and jump ratios for 30 elements between Ti ( Z = 22) and Er ( Z = 68) were measured by energy dispersive X-ray fluorescence (EDXRF) technique. The jump factors and jump ratios for these elements were determined by measuring the K shell fluorescence parameters such as the Kα X-ray production cross-sections, K shell fluorescence yields, Kβ-to- Kα X-rays intensity ratios, total atomic absorption cross sections and mass attenuation coefficients. The measurements were performed using an Am-241 radioactive point source and a Si (Li) detector in direct excitation and transmission experimental geometry. The results for jump factors and jump ratios were compared with theoretically calculated and the ones available in the literature.

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

Development of a spectro-electrochemical cell for soft X-ray photon-in photon-out spectroscopy

NASA Astrophysics Data System (ADS)

Ishihara, Tomoko; Tokushima, Takashi; Horikawa, Yuka; Kato, Masaru; Yagi, Ichizo

2017-10-01

We developed a spectro-electrochemical cell for X-ray absorption and X-ray emission spectroscopy, which are element-specific methods to study local electronic structures in the soft X-ray region. In the usual electrochemical measurement setup, the electrode is placed in solution, and the surface/interface region of the electrode is not normally accessible by soft X-rays that have low penetration depth in liquids. To realize soft X-ray observation of electrochemical reactions, a 15-nm-thick Pt layer was deposited on a 150-nm-thick film window with an adhesive 3-nm-thick Ti layer for use as both the working electrode and the separator window between vacuum and a sample liquid under atmospheric pressure. The designed three-electrode electrochemical cell consists of a Pt film on a SiC window, a platinized Pt wire, and a commercial Ag|AgCl electrode as the working, counter, and reference electrodes, respectively. The functionality of the cell was tested by cyclic voltammetry and X-ray absorption and emission spectroscopy. As a demonstration, the electroplating of Pb on the Pt/SiC membrane window was measured by X-ray absorption and real-time monitoring of fluorescence intensity at the O 1s excitation.

A Wireless Sensor Network for Growth Environment Measurement and Multi-Band Optical Sensing to Diagnose Tree Vigor

PubMed Central

Kameoka, Shinichi; Isoda, Shuhei; Hashimoto, Atsushi; Ito, Ryoei; Miyamoto, Satoru; Wada, Genki; Watanabe, Naoki; Yamakami, Takashi; Suzuki, Ken; Kameoka, Takaharu

2017-01-01

We have tried to develop the guidance system for farmers to cultivate using various phenological indices. As the sensing part of this system, we deployed a new Wireless Sensor Network (WSN). This system uses the 920 MHz radio wave based on the Wireless Smart Utility Network that enables long-range wireless communication. In addition, the data acquired by the WSN were standardized for the advanced web service interoperability. By using these standardized data, we can create a web service that offers various kinds of phenological indices as secondary information to the farmers in the field. We have also established the field management system using thermal image, fluorescent and X-ray fluorescent methods, which enable the nondestructive, chemical-free, simple, and rapid measurement of fruits or trees. We can get the information about the transpiration of plants through a thermal image. The fluorescence sensor gives us information, such as nitrate balance index (NBI), that shows the nitrate balance inside the leaf, chlorophyll content, flavonol content and anthocyanin content. These methods allow one to quickly check the health of trees and find ways to improve the tree vigor of weak ones. Furthermore, the fluorescent x-ray sensor has the possibility to quantify the loss of minerals necessary for fruit growth. PMID:28448452

A Wireless Sensor Network for Growth Environment Measurement and Multi-Band Optical Sensing to Diagnose Tree Vigor.

PubMed

Kameoka, Shinichi; Isoda, Shuhei; Hashimoto, Atsushi; Ito, Ryoei; Miyamoto, Satoru; Wada, Genki; Watanabe, Naoki; Yamakami, Takashi; Suzuki, Ken; Kameoka, Takaharu

2017-04-27

We have tried to develop the guidance system for farmers to cultivate using various phenological indices. As the sensing part of this system, we deployed a new Wireless Sensor Network (WSN). This system uses the 920 MHz radio wave based on the Wireless Smart Utility Network that enables long-range wireless communication. In addition, the data acquired by the WSN were standardized for the advanced web service interoperability. By using these standardized data, we can create a web service that offers various kinds of phenological indices as secondary information to the farmers in the field. We have also established the field management system using thermal image, fluorescent and X-ray fluorescent methods, which enable the nondestructive, chemical-free, simple, and rapid measurement of fruits or trees. We can get the information about the transpiration of plants through a thermal image. The fluorescence sensor gives us information, such as nitrate balance index (NBI), that shows the nitrate balance inside the leaf, chlorophyll content, flavonol content and anthocyanin content. These methods allow one to quickly check the health of trees and find ways to improve the tree vigor of weak ones. Furthermore, the fluorescent x-ray sensor has the possibility to quantify the loss of minerals necessary for fruit growth.

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

Discrimination and quantification of Fe and Ni abundances in Genesis solar wind implanted collectors using X-ray standing wave fluorescence yield depth profiling with internal referencing

DOE PAGES

Choi, Y.; Eng, P.; Stubbs, J.; ...

2016-08-21

In this paper, X-ray standing wave fluorescence yield depth profiling was used to determine the solar wind implanted Fe and Ni fluences in a silicon-on-sapphire (SoS) Genesis collector (60326). An internal reference standardization method was developed based on fluorescence from Si and Al in the collector materials. Measured Fe fluence agreed well with that measured previously by us on a sapphire collector (50722) as well as SIMS results by Jurewicz et al. Measured Ni fluence was higher than expected by a factor of two; neither instrumental errors nor solar wind fractionation effects are considered significant perturbations to this value. Impuritymore » Ni within the epitaxial Si layer, if present, could explain the high Ni fluences and therefore needs further investigation. As they stand, these results are consistent with minor temporally-variable Fe and Ni fractionation on the timescale of a year.« less

Discrimination and quantification of Fe and Ni abundances in Genesis solar wind implanted collectors using X-ray standing wave fluorescence yield depth profiling with internal referencing

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

Choi, Y.; Eng, P.; Stubbs, J.

In this paper, X-ray standing wave fluorescence yield depth profiling was used to determine the solar wind implanted Fe and Ni fluences in a silicon-on-sapphire (SoS) Genesis collector (60326). An internal reference standardization method was developed based on fluorescence from Si and Al in the collector materials. Measured Fe fluence agreed well with that measured previously by us on a sapphire collector (50722) as well as SIMS results by Jurewicz et al. Measured Ni fluence was higher than expected by a factor of two; neither instrumental errors nor solar wind fractionation effects are considered significant perturbations to this value. Impuritymore » Ni within the epitaxial Si layer, if present, could explain the high Ni fluences and therefore needs further investigation. As they stand, these results are consistent with minor temporally-variable Fe and Ni fractionation on the timescale of a year.« less

Fluorescence and physical properties of the organic salt 2-chloro-4-nitrobenzoate-3-ammonium-phenol

NASA Astrophysics Data System (ADS)

Mani, Rajaboopathi; Rietveld, Ivo B.; Nicolaï, Béatrice; Varadharajan, Krishnakumar; Louhi-Kultanen, Marjatta; Narasimhan, Surumbarkuzhali

2015-09-01

Organic salt 2-chloro-4-nitrobenzoate (CNBA-) 3-ammonium-phenol (AP+) exhibits fluorescence at 338 nm in solution and frontier molecular orbitals generated from TDDFT calculations indicate that the ground state and the excited state are physically separated on AP+ and CNBA-. The crystal structure and physical-chemical properties of the CNBA- · AP+ were investigated using X-ray single crystal and powder diffraction, SEM, FTIR, UV-Vis-NIR, and fluorescence spectrometry. X-ray diffraction demonstrates that the two molecules are linked via N+-H⋯O- ammonium-carboxylate interactions, as expected considering their interaction propensities. Proton transfer has been confirmed by FTIR analysis. The melting point of CNBA- · AP+ was observed at 186 °C, which is higher than pure CNBA (140 °C) or AP (120 °C). The observation of a spatially separated HOMO and LUMO possessing a narrow ΔEST = 73.3 meV and an emission in the blue region is promising as an alternative method for the production of OLED materials.

FMT-XCT: in vivo animal studies with hybrid fluorescence molecular tomography-X-ray computed tomography.

PubMed

Ale, Angelique; Ermolayev, Vladimir; Herzog, Eva; Cohrs, Christian; de Angelis, Martin Hrabé; Ntziachristos, Vasilis

2012-06-01

The development of hybrid optical tomography methods to improve imaging performance has been suggested over a decade ago and has been experimentally demonstrated in animals and humans. Here we examined in vivo performance of a camera-based hybrid fluorescence molecular tomography (FMT) system for 360° imaging combined with X-ray computed tomography (XCT). Offering an accurately co-registered, information-rich hybrid data set, FMT-XCT has new imaging possibilities compared to stand-alone FMT and XCT. We applied FMT-XCT to a subcutaneous 4T1 tumor mouse model, an Aga2 osteogenesis imperfecta model and a Kras lung cancer mouse model, using XCT information during FMT inversion. We validated in vivo imaging results against post-mortem planar fluorescence images of cryoslices and histology data. Besides offering concurrent anatomical and functional information, FMT-XCT resulted in the most accurate FMT performance to date. These findings indicate that addition of FMT optics into the XCT gantry may be a potent upgrade for small-animal XCT systems.

Determination of the Mass Absorption Coefficient in Two-Layer Ti/V and V/Ti Thin Film Systems by the X-Ray Fluorescence Method

NASA Astrophysics Data System (ADS)

Mashin, N. I.; Chernyaeva, E. A.; Tumanova, A. N.; Gafarova, L. M.

2016-03-01

A new XRF procedure for the determination of the mass absorption coefficient in thin film Ti/V and V/Ti two-layer systems has been proposed. The procedure uses easy-to-make thin-film layers of sputtered titanium and vanadium on a polymer film substrate. Correction coefficients have been calculated that take into account attenuation of primary radiation of the X-ray tube, as well as attenuation of the spectral line of the bottom layer element in the top layer.

High-Resolution Detector For X-Ray Diffraction

NASA Technical Reports Server (NTRS)

Carter, Daniel C.; Withrow, William K.; Pusey, Marc L.; Yost, Vaughn H.

1988-01-01

Proposed x-ray-sensitive imaging detector offers superior spatial resolution, counting-rate capacity, and dynamic range. Instrument based on laser-stimulated luminescence and reusable x-ray-sensitive film. Detector scans x-ray film line by line. Extracts latent image in film and simultaneously erases film for reuse. Used primarily for protein crystallography. Principle adapted to imaging detectors for electron microscopy and fluorescence spectroscopy and general use in astronomy, engineering, and medicine.

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.

Superior spatial resolution in confocal X-ray techniques using collimating channel array optics: elemental mapping and speciation in archaeological human bone

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

Choudhury, S.; Agyeman-Budu, D. N.; Woll, A. R.

Confocal X-ray fluorescence imaging (CXFI) and confocal X-ray absorption spectroscopy (CXAS) respectively enable the study of three dimensionally resolved localization and speciation of elements. Applied to a thick sample, essentially any volume element of interest within the X-ray fluorescence escape depth can be examined without the need for physical thin sectioning. To date, X-ray confocal detection generally has employed a polycapillary optic in front of the detector to collect fluorescence from the probe volume formed at the intersection of its focus with the incident microfocus beam. This work demonstrates the capability of a novel Collimating Channel Array (CCA) optic inmore » providing an improved and essentially energy independent depth resolution approaching 2 μm. By presenting a comparison of elemental maps of archaeological bone collected without confocal detection, and with polycapillary- and CCA-based confocal detection, this study highlights the strengths and limitations of each mode. Unlike the polycapillary, the CCA shows similar spatial resolution in maps for both low (Ca) and high (Pb and Sr) energy X-ray fluorescence, thus illustrating the energy independent nature of the CCA optic resolution. While superior spatial resolution is demonstrated for all of these elements, the most significant improvement is observed for Ca, demonstrating the advantage of employing the CCA optic in examining light elements. In addition to CXFI, this configuration also enables the collection of Pb L3 CXAS data from micro-volumes with dimensions comparable to bone microstructures of interest. Our CXAS result, which represents the first CCA-based biological CXAS, demonstrates the ability of CCA optics to collect site specific spectroscopic information. The demonstrated combination of site-specific elemental localization and speciation data will be useful in diverse fields.« 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

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND ROUTINE USE OF THE SPECTRACE 9000 FIELD PORTABLE X-RAY FLUORESCENCE ANALYZER (UA-L-10.1)

EPA Science Inventory

The purpose of this SOP is to describe the procedures for operating and calibrating the Spectrace 9000 field portable X-ray fluorescence analyzer. This procedure applies to the determination of metal concentrations in samples during the Arizona NHEXAS project and the Border stud...

Discovery of Oxygen Kalpha X-ray Emission from the Rings of Saturn

NASA Technical Reports Server (NTRS)

Bhardwaj, Anil; Elsner, Ronald F.; Waite, J. Hunter, Jr.; Gladstone, G Randall; Cravens, Thomas E.; Ford, Peter G.

2005-01-01

Using the Advanced CCD Imaging Spectrometer (ACIS), the Chandra X-ray Observatory (CXO) observed the Saturnian system for one rotation of the planet (approx.37 ks) on 20 January, 2004, and again on 26-27 January, 2004. In this letter we report the detection of X-ray emission from the rings of Saturn. The X-ray spectrum from the rings is dominated by emission in a narrow (approx.130 eV wide) energy band centered on the atomic oxygen Ka fluorescence line at 0.53 keV. The X-ray power emitted from the rings in the 0.49-0.62 keV band is about one-third of that emitted from Saturn disk in the photon energy range 0.24-2.0 keV. Our analysis also finds a clear detection of X-ray emission from the rings in the 0.49-0.62 keV band in an earlier (14-15 April, 2003) Chandra ACIS observation of Saturn. Fluorescent scattering of solar X-rays from oxygen atoms in the H20 icy ring material is the likely source mechanism for ring X-rays, consistent with the scenario of solar photo-production of a tenuous ring oxygen atmosphere and ionosphere recently discovered by Cassini.

An IAEA multi-technique X-ray spectrometry endstation at Elettra Sincrotrone Trieste: benchmarking results and interdisciplinary applications.

PubMed

Karydas, Andreas Germanos; Czyzycki, Mateusz; Leani, Juan José; Migliori, Alessandro; Osan, Janos; Bogovac, Mladen; Wrobel, Pawel; Vakula, Nikita; Padilla-Alvarez, Roman; Menk, Ralf Hendrik; Gol, Maryam Ghahremani; Antonelli, Matias; Tiwari, Manoj K; Caliri, Claudia; Vogel-Mikuš, Katarina; Darby, Iain; Kaiser, Ralf Bernd

2018-01-01

The International Atomic Energy Agency (IAEA) jointly with the Elettra Sincrotrone Trieste (EST) operates a multipurpose X-ray spectrometry endstation at the X-ray Fluorescence beamline (10.1L). The facility has been available to external users since the beginning of 2015 through the peer-review process of EST. Using this collaboration framework, the IAEA supports and promotes synchrotron-radiation-based research and training activities for various research groups from the IAEA Member States, especially those who have limited previous experience and resources to access a synchrotron radiation facility. This paper aims to provide a broad overview about various analytical capabilities, intrinsic features and performance figures of the IAEA X-ray spectrometry endstation through the measured results. The IAEA-EST endstation works with monochromatic X-rays in the energy range 3.7-14 keV for the Elettra storage ring operating at 2.0 or 2.4 GeV electron energy. It offers a combination of different advanced analytical probes, e.g. X-ray reflectivity, X-ray absorption fine-structure measurements, grazing-incidence X-ray fluorescence measurements, using different excitation and detection geometries, and thereby supports a comprehensive characterization for different kinds of nanostructured and bulk materials.

Quantitative X-ray mapping, scatter diagrams and the generation of correction maps to obtain more information about your material

NASA Astrophysics Data System (ADS)

Wuhrer, R.; Moran, K.

2014-03-01

Quantitative X-ray mapping with silicon drift detectors and multi-EDS detector systems have become an invaluable analysis technique and one of the most useful methods of X-ray microanalysis today. The time to perform an X-ray map has reduced considerably with the ability to map minor and trace elements very accurately due to the larger detector area and higher count rate detectors. Live X-ray imaging can now be performed with a significant amount of data collected in a matter of minutes. A great deal of information can be obtained from X-ray maps. This includes; elemental relationship or scatter diagram creation, elemental ratio mapping, chemical phase mapping (CPM) and quantitative X-ray maps. In obtaining quantitative x-ray maps, we are able to easily generate atomic number (Z), absorption (A), fluorescence (F), theoretical back scatter coefficient (η), and quantitative total maps from each pixel in the image. This allows us to generate an image corresponding to each factor (for each element present). These images allow the user to predict and verify where they are likely to have problems in our images, and are especially helpful to look at possible interface artefacts. The post-processing techniques to improve the quantitation of X-ray map data and the development of post processing techniques for improved characterisation are covered in this paper.

HIGH-RESOLUTION X-RAY SPECTROSCOPY REVEALS THE SPECIAL NATURE OF WOLF-RAYET STAR WINDS

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

Oskinova, L. M.; Hamann, W.-R.; Gayley, K. G.

We present the first high-resolution X-ray spectrum of a putatively single Wolf-Rayet (WR) star. 400 ks observations of WR 6 by the XMM-Newton telescope resulted in a superb quality high-resolution X-ray spectrum. Spectral analysis reveals that the X-rays originate far out in the stellar wind, more than 30 stellar radii from the photosphere, and thus outside the wind acceleration zone where the line-driving instability (LDI) could create shocks. The X-ray emitting plasma reaches temperatures up to 50 MK and is embedded within the unshocked, 'cool' stellar wind as revealed by characteristic spectral signatures. We detect a fluorescent Fe line atmore » Almost-Equal-To 6.4 keV. The presence of fluorescence is consistent with a two-component medium, where the cool wind is permeated with the hot X-ray emitting plasma. The wind must have a very porous structure to allow the observed amount of X-rays to escape. We find that neither the LDI nor any alternative binary scenario can explain the data. We suggest a scenario where X-rays are produced when the fast wind rams into slow 'sticky clumps' that resist acceleration. Our new data show that the X-rays in single WR star are generated by some special mechanism different from the one operating in the O-star winds.« less

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.

Spatiotemporal Monte Carlo transport methods in x-ray semiconductor detectors: application to pulse-height spectroscopy in a-Se.

PubMed

Fang, Yuan; Badal, Andreu; Allec, Nicholas; Karim, Karim S; Badano, Aldo

2012-01-01

The authors describe a detailed Monte Carlo (MC) method for the coupled transport of ionizing particles and charge carriers in amorphous selenium (a-Se) semiconductor x-ray detectors, and model the effect of statistical variations on the detected signal. A detailed transport code was developed for modeling the signal formation process in semiconductor x-ray detectors. The charge transport routines include three-dimensional spatial and temporal models of electron-hole pair transport taking into account recombination and trapping. Many electron-hole pairs are created simultaneously in bursts from energy deposition events. Carrier transport processes include drift due to external field and Coulombic interactions, and diffusion due to Brownian motion. Pulse-height spectra (PHS) have been simulated with different transport conditions for a range of monoenergetic incident x-ray energies and mammography radiation beam qualities. Two methods for calculating Swank factors from simulated PHS are shown, one using the entire PHS distribution, and the other using the photopeak. The latter ignores contributions from Compton scattering and K-fluorescence. Comparisons differ by approximately 2% between experimental measurements and simulations. The a-Se x-ray detector PHS responses simulated in this work include three-dimensional spatial and temporal transport of electron-hole pairs. These PHS were used to calculate the Swank factor and compare it with experimental measurements. The Swank factor was shown to be a function of x-ray energy and applied electric field. Trapping and recombination models are all shown to affect the Swank factor.

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.

The superconducting high-resolution soft X-ray spectrometer at the advanced biological and environmental X-ray facility

NASA Astrophysics Data System (ADS)

Friedrich, S.; Drury, O. B.; George, S. J.; Cramer, S. P.

2007-11-01

We have built a 36-pixel superconducting tunnel junction X-ray spectrometer for chemical analysis of dilute samples in the soft X-ray band. It offers an energy resolution of ˜10-20 eV FWHM below 1 keV, a solid angle coverage of ˜10 -3, and can be operated at total rates of up to ˜10 6 counts/s. Here, we describe the spectrometer performance in speciation measurements by fluorescence-detected X-ray absorption spectroscopy at the Advanced Biological and Environmental X-ray facility at the ALS synchrotron.

Fast fluorescence techniques for crystallography beamlines

PubMed Central

Stepanov, Sergey; Hilgart, Mark; Yoder, Derek W.; Makarov, Oleg; Becker, Michael; Sanishvili, Ruslan; Ogata, Craig M.; Venugopalan, Nagarajan; Aragão, David; Caffrey, Martin; Smith, Janet L.; Fischetti, Robert F.

2011-01-01

This paper reports on several developments of X-ray fluorescence techniques for macromolecular crystallography recently implemented at the National Institute of General Medical Sciences and National Cancer Institute beamlines at the Advanced Photon Source. These include (i) three-band on-the-fly energy scanning around absorption edges with adaptive positioning of the fine-step band calculated from a coarse pass; (ii) on-the-fly X-ray fluorescence rastering over rectangular domains for locating small and invisible crystals with a shuttle-scanning option for increased speed; (iii) fluorescence rastering over user-specified multi-segmented polygons; and (iv) automatic signal optimization for reduced radiation damage of samples. PMID:21808424

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 Silicon as well as Arsenic implants in Silicon. The results of the different optimization algorithms have been compared to test the convergence of the algorithms. Finally, simulations for Iron nanoparticles on bulk Silicon and on a W/C multilayer are presented, using the assumption of an unaltered X-ray Standing Wave above the surface.

Green synthesis of carbon dots originated from Lycii Fructus for effective fluorescent sensing of ferric ion and multicolor cell imaging.

PubMed

Sun, Xiaohan; He, Jiang; Yang, Shenghong; Zheng, Mingda; Wang, Yingying; Ma, Shuang; Zheng, Haipeng

2017-10-01

Green, economical and effective method was developed for synthesis of fluorescent carbon dots (CDs), using one-pot hydrothermal treatment of Lycii Fructus. Optical and structural properties of the CDs have been extensively studied by UV-visible and fluorescence spectroscopic, x-ray diffraction (XRD) techniques, transmission electron microscopy (TEM) and high resolution TEM (HRTEM). Surface functionality and composition of CDs has been illustrated by Fourier transform infrared spectroscopy (FTIR), x-ray photoelectron spectroscopy (XPS) spectra and elemental analysis. The fabricated CDs possess stable fluorescent properties. The fluorescent quantum yield of the CDs can reach 17.2%. The prepared CDs emitted a broad fluorescence between 415 and 545nm and their fluorescence was tuned by changing excitation wavelength. Meanwhile, the fluorescence intensity of the CDs could be significantly quenched by Fe 3+ (turn-off). The CDs exhibit captivating sensitivity and selectivity toward Fe 3+ with a linear range from 0 to 30μM and a detection limit of 21nM. The prepared CDs were successfully applied to the determination of Fe 3+ in the urine samples, the water samples from the from the Yellow River and living HeLa (Henrietta Lacks) cells. Moreover, the low-toxicity and excellent biocompatibility of the CDs were evaluated through MTT assay on HeLa cells. The CDs were also employed as fluorescent probes for multicolor imaging of HeLa cells successfully. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of Zn/Cu ratio and oligoelements in serum samples by total reflection X-ray fluorescence spectrometry for cancer diagnosis

NASA Astrophysics Data System (ADS)

Marcó P., L. M.; Jiménez, E.; Hernández C., E. A.; Rojas, A.; Greaves, E. D.

2001-11-01

The method of quantification using the Compton peak as an internal standard, developed in a previous work, was applied to the routine determination of Fe, Cu, Zn and Se in serum samples from normal individuals and cancer patients by total reflection X-ray fluorescence spectrometry. Samples were classified according to age and sex of the donor, in order to determine reference values for normal individuals. Results indicate that the Zn/Cu ratio and the Cu concentration could prove to be useful tools for cancer diagnosis. Significant differences in these parameters between the normal and cancer group were found for all age ranges. The multielemental character of the technique, coupled with the small amounts of sample required and the short analysis time make it a valuable tool in clinical analysis.

X-ray fluorescence at nanoscale resolution for multicomponent layered structures: A solar cell case study

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

West, Bradley M.; Stuckelberger, Michael; Jeffries, April

The study of a multilayered and multicomponent system by spatially resolved X-ray fluorescence microscopy poses unique challenges in achieving accurate quantification of elemental distributions. This is particularly true for the quantification of materials with high X-ray attenuation coefficients, depth-dependent composition variations and thickness variations. A widely applicable procedure for use after spectrum fitting and quantification is described. This procedure corrects the elemental distribution from the measured fluorescence signal, taking into account attenuation of the incident beam and generated fluorescence from multiple layers, and accounts for sample thickness variations. Deriving from Beer–Lambert's law, formulae are presented in a general integral formmore » and numerically applicable framework. Here, the procedure is applied using experimental data from a solar cell with a Cu(In,Ga)Se 2 absorber layer, measured at two separate synchrotron beamlines with varied measurement geometries. This example shows the importance of these corrections in real material systems, which can change the interpretation of the measured distributions dramatically.« less

X-ray fluorescence at nanoscale resolution for multicomponent layered structures: A solar cell case study

DOE PAGES

West, Bradley M.; Stuckelberger, Michael; Jeffries, April; ...

2017-01-01

The study of a multilayered and multicomponent system by spatially resolved X-ray fluorescence microscopy poses unique challenges in achieving accurate quantification of elemental distributions. This is particularly true for the quantification of materials with high X-ray attenuation coefficients, depth-dependent composition variations and thickness variations. A widely applicable procedure for use after spectrum fitting and quantification is described. This procedure corrects the elemental distribution from the measured fluorescence signal, taking into account attenuation of the incident beam and generated fluorescence from multiple layers, and accounts for sample thickness variations. Deriving from Beer–Lambert's law, formulae are presented in a general integral formmore » and numerically applicable framework. Here, the procedure is applied using experimental data from a solar cell with a Cu(In,Ga)Se 2 absorber layer, measured at two separate synchrotron beamlines with varied measurement geometries. This example shows the importance of these corrections in real material systems, which can change the interpretation of the measured distributions dramatically.« less

Comet composition and density analyzer

NASA Technical Reports Server (NTRS)

Clark, B. C.

1982-01-01

Distinctions between cometary material and other extraterrestrial materials (meteorite suites and stratospherically-captured cosmic dust) are addressed. The technique of X-ray fluorescence (XRF) for analysis of elemental composition is involved. Concomitant with these investigations, the problem of collecting representative samples of comet dust (for rendezvous missions) was solved, and several related techniques such as mineralogic analysis (X-ray diffraction), direct analysis of the nucleus without docking (electron macroprobe), dust flux rate measurement, and test sample preparation were evaluated. An explicit experiment concept based upon X-ray fluorescence analysis of biased and unbiased sample collections was scoped and proposed for a future rendezvous mission with a short-period comet.

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

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

NASA Technical Reports Server (NTRS)

Leonard, R. F.

1977-01-01

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

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.

Fluorescence x-ray absorption fine structure studies of Fe-Ni-S and Fe-Ni-Si melts to 1600 K

NASA Astrophysics Data System (ADS)

Manghnani, M. H.; Hong, X.; Balogh, J.; Amulele, G.; Sekar, M.; Newville, M.

2008-04-01

We report NiK -edge fluorescence x-ray absorption fine structure spectra (XAFS) for Fe0.75Ni0.05S0.20 and Fe0.75Ni0.05Si0.20 ternary alloys from room temperature up to 1600 K. A high-temperature furnace designed for these studies incorporates two x-ray transparent windows and enables both a vertical orientation of the molten sample and a wide opening angle, so that XAFS can be measured in the fluorescence mode with a detector at 90° with respect to the incident x-ray beam. An analysis of the Ni XAFS data for these two alloys indicates different local structural environments for Ni in Fe0.75Ni0.05S0.20 and Fe0.75Ni0.05Si0.20 melts, with more Ni-Si coordination than Ni-S coordination persisting from room temperature through melting. These results suggest that light elements such as S and Si may impact the structural and chemical properties of Fe-Ni alloys with a composition similar to the earth’s core.

Asphalt-Aggregate Interactions in Hot Recycling.

DTIC Science & Technology

1987-07-01

Mexico Powders and Granular Materials Laboratory for surface area/porosity measurements and discussion of results John Husler and Les Mcfadden at the...Alamos National Laboratory by X-Ray Fluorescence," LA-96630Ms, May, 1983. 29. Husler , J., "Standard Laboratory Methods for the Chemical Analysis of

Recovering Ancient Inscriptions by X-ray Fluorescence Imaging

NASA Astrophysics Data System (ADS)

Powers, Judson; Dimitrova, Nora; Huang, Rong; Smilgies, Detlef-M.; Bilderback, Don; Clinton, Kevin; Thorne, Robert

2006-03-01

For many ancient cultures including those of the Mediterranean, carved stone inscriptions provide our most detailed historical record. Over the ages the surfaces of many of these inscriptions have been eroded so that the original text can no longer be distinguished. A method that allowed at least partial recovery of this lost text would provide a major breakthrough for the study of these cultures. The scope of analytical techniques that can be applied to stone tablets is limited by their large size and weight. We have applied X-ray fluorescence imaging to study the text of ancient stone inscriptions [1]. This method allows the concentrations of trace elements, including those introduced during inscription and painting, to be measured and mapped. The images created in this way correspond exactly to the published text of the inscription, both when traces of letters are visible with the naked eye and when they are barely detectable. [1] J. Powers et al., Zeitschrift für Papyrologie und Epigraphik 152: 221-227 (2005).

Generation of the additional fluorescence radiation in the elastomeric shields used in computer tomography (CT).

PubMed

Szajerski, P; Zaborski, M; Bem, H; Baryn, W; Kusiak, E

Two commercially available (EP, Z) and eight new elastomeric composites (M1-M4, G1-G4, of thickness ≈1 mm) containing mixtures of differing proportions of heavy metal additives (Bi, W, Gd and Sb) have been synthesised and examined as protective shields. The intensity of the X-ray fluorescence radiation generated in the typical elastomeric shields for CT, containing Bi and other heavy metal additives influence on the practical shielding properties. A method for assessing the radiation shielding properties of elastomeric composites used in CT examination procedures via X-ray spectrometry has been proposed. To measure the radiation reduction ability of the protective shields, the dose reduction factor (DRF) has been determined. The lead equivalents for the examined composites were within the ranges of 0.046-0.128 and 0.048-0.130 mm for 122.1 and 136.5 keV photons, respectively. The proposed method, unlike to the common approach, includes a dose contribution from the induced X-ray fluorescence radiation of the heavy metal elements in the protective shields. The results clearly indicate that among the examined compositions, the highest values DRF have been achieved with preparations containing Bi+W, Bi+W+Gd and Bi+W+Sb mixtures with gradually decreasing content of heavy metal additives in the following order: Bi, W, Gd and Sb. The respective values of DRF obtained for the investigated composites were 21, 28 and 27 % dose reduction for a 1 mm thick shield and 39 and ~50 % for a 2 mm thick layer (M1-M4).

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…

Tracking ink composition on Herculaneum papyrus scrolls: quantification and speciation of lead by X-ray based techniques and Monte Carlo simulations

PubMed Central

Tack, Pieter; Cotte, Marine; Bauters, Stephen; Brun, Emmanuel; Banerjee, Dipanjan; Bras, Wim; Ferrero, Claudio; Delattre, Daniel; Mocella, Vito; Vincze, Laszlo

2016-01-01

The writing in carbonized Herculaneum scrolls, covered and preserved by the pyroclastic events of the Vesuvius in 79 AD, was recently revealed using X-ray phase-contrast tomography, without the need of unrolling the sensitive scrolls. Unfortunately, some of the text is difficult to read due to the interference of the papyrus fibers crossing the written text vertically and horizontally. Recently, lead was found as an elemental constituent in the writing, rendering the text more clearly readable when monitoring the lead X-ray fluorescence signal. Here, several hypotheses are postulated for the origin and state of lead in the papyrus writing. Multi-scale X-ray fluorescence micro-imaging, Monte Carlo quantification and X-ray absorption microspectroscopy experiments are used to provide additional information on the ink composition, in an attempt to determine the origin of the lead in the Herculaneum scrolls and validate the postulated hypotheses. PMID:26854067

NBSGSC - a FORTRAN program for quantitative x-ray fluorescence analysis. Technical note (final)

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

Tao, G.Y.; Pella, P.A.; Rousseau, R.M.

1985-04-01

A FORTRAN program (NBSGSC) was developed for performing quantitative analysis of bulk specimens by x-ray fluorescence spectrometry. This program corrects for x-ray absorption/enhancement phenomena using the comprehensive alpha coefficient algorithm proposed by Lachance (COLA). NBSGSC is a revision of the program ALPHA and CARECAL originally developed by R.M. Rousseau of the Geological Survey of Canada. Part one of the program (CALCO) performs the calculation of theoretical alpha coefficients, and part two (CALCOMP) computes the composition of the analyte specimens. The analysis of alloys, pressed minerals, and fused specimens can currently be treated by the program. In addition to using measuredmore » x-ray tube spectral distributions, spectra from seven commonly used x-ray tube targets could also be calculated with an NBS algorithm included in the program. NBSGSC is written in FORTRAN IV for a Digital Equipment Corporation (DEC PDP-11/23) minicomputer using RLO2 firm disks and an RSX 11M operating system.« less

Beamline 10.3.2 at ALS: a hard X-ray microprobe for environmental and materials sciences.

PubMed

Marcus, Matthew A; MacDowell, Alastair A; Celestre, Richard; Manceau, Alain; Miller, Tom; Padmore, Howard A; Sublett, Robert E

2004-05-01

Beamline 10.3.2 at the ALS is a bend-magnet line designed mostly for work on environmental problems involving heavy-metal speciation and location. It offers a unique combination of X-ray fluorescence mapping, X-ray microspectroscopy and micro-X-ray diffraction. The optics allow the user to trade spot size for flux in a size range of 5-17 microm in an energy range of 3-17 keV. The focusing uses a Kirkpatrick-Baez mirror pair to image a variable-size virtual source onto the sample. Thus, the user can reduce the effective size of the source, thereby reducing the spot size on the sample, at the cost of flux. This decoupling from the actual source also allows for some independence from source motion. The X-ray fluorescence mapping is performed with a continuously scanning stage which avoids the time overhead incurred by step-and-repeat mapping schemes. The special features of this beamline are described, and some scientific results shown.

Study of Cr/Sc-based multilayer reflecting mirrors using soft x-ray reflectivity and standing wave-enhanced x-ray fluorescence

NASA Astrophysics Data System (ADS)

Wu, Meiyi; Burcklen, Catherine; André, Jean-Michel; Guen, Karine Le; Giglia, Angelo; Koshmak, Konstantin; Nannarone, Stefano; Bridou, Françoise; Meltchakov, Evgueni; Rossi, Sébastien de; Delmotte, Franck; Jonnard, Philippe

2017-11-01

We study Cr/Sc-based multilayer mirrors designed to work in the water window range using hard and soft x-ray reflectivity as well as x-ray fluorescence enhanced by standing waves. Samples differ by the elemental composition of the stack, the thickness of each layer, and the order of deposition. This paper mainly consists of two parts. In the first part, the optical performances of different Cr/Sc-based multilayers are reported, and in the second part, we extend further the characterization of the structural parameters of the multilayers, which can be extracted by comparing the experimental data with simulations. The methodology is detailed in the case of Cr/B4C/Sc sample for which a three-layer model is used. Structural parameters determined by fitting reflectivity curve are then introduced as fixed parameters to plot the x-ray standing wave curve, to compare with the experiment, and confirm the determined structure of the stack.

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

NASA Astrophysics Data System (ADS)

Nikonow, Wilhelm; Rammlmair, Dieter

2016-11-01

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

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.

The hoard of Beçin—non-destructive analysis of the silver coins

NASA Astrophysics Data System (ADS)

Rodrigues, M.; Schreiner, M.; Mäder, M.; Melcher, M.; Guerra, M.; Salomon, J.; Radtke, M.; Alram, M.; Schindel, N.

2010-05-01

We report the results of an analytical investigation on 416 silver-copper coins stemming from the Ottoman Empire (end of 16th and beginning of 17th centuries), using synchrotron micro X-ray fluorescence analysis (SRXRF). In the past, analyses had already been conducted with energy dispersive X-ray fluorescence analysis (EDXRF), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM/EDX) and proton induced X-ray emission spectroscopy (PIXE). With this combination of techniques it was possible to confirm the fineness of the coinage as well as to study the provenance of the alloy used for the coins. For the interpretation of the data statistical analysis (principal component analysis—PCA) has been performed. A definite local assignment was explored and significant clustering was obtained regarding the minor and trace elements composing the coin alloys.

Problems in determination of skeletal lead burden in archaeological samples: An example from the First African Baptist Church population

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

Whittmers Jr., L. E.; Aufderheide, A. C.; Pounds, Joel G.

2008-08-01

Human bone lead content has been demonstrated to be related to socioeconomic status, occupation and other social and environmental correlates. Skeletal tissue samples from 135 individuals from an early nineteenth century Philadelphia cemetery (First African Baptist Church) were studied by electrothermal atomic absorption spectrometry and x-ray fluorescence for lead content. High bone lead levels led to investigation of possible diagenetic effects. These were investigated by several different approaches including distribution of lead within bone by x-ray fluorescence, histological preservation, soil lead concentration and acidity as well as location and depth of burial. Bone lead levels were very high in themore » children, exceeding those of the adult population that were buried in the cemetery, and also those of present day adults. The antemortem age-related increase in bone lead, reported in other studies, was not evidenced in this population. Lead was even deposited in areas of taphonomic bone destruction. Synchrotron x-ray fluorescence studies revealed no consistent pattern of lead microdistribution within the bone. Our conclusions are that postmortem diagenesis of lead ion has penetrated these archaeological bones to a degree that makes their original bone lead content irretrievable by any known method. Increased bone porosity is most likely responsible for the very high levels of lead found in bones of newborns and children.« less

Problems in Determination of Skeletal Lead Burden in Archaeological Samples: An Example From the First African Baptist Church Population

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

Whittmers Jr., L. E.; Aufderheide, A. C.; Pounds, Joel G.

2008-08-01

ABSTRACT Human bone lead content has been demonstrated to be related to socioeconomic status, occupation and other social and environmental correlates. Skeletal tissue samples from 135 individuals from an early nineteenth century Philadelphia cemetery (First African Baptist Church) were studied by electrothermal atomic absorption spectrometry and x-ray fluorescence for lead content. High bone lead levels led to investigation of possible diagenetic effects. These were investigated by several different approaches including distribution of lead within bone by x-ray fluorescence, histological preservation, soil lead concentration and acidity as well as location and depth of burial. Bone lead levels were very high inmore » children, exceeding those of the adult population that were buried in the cemetery, and also those of present day adults. The antemortem age-related increase in bone lead, reported in other studies, was not evidenced in this population. Lead was even deposited in areas of taphonomic bone destruction. Synchrotron x-ray fluorescence studies revealed no consistent pattern of lead microdistribution within the bone. Our conclusions are that postmortem diagenesis of lead ion has penetrated these archaeological bones to a degree that makes their original bone lead content irretrievable by any known method. Increased bone porosity is most likely responsible for the very high levels of lead found in bones of newborns and children.« less

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.

Theoretical study of depth profiling with gamma- and X-ray spectrometry based on measurements of intensity ratios

NASA Astrophysics Data System (ADS)

Bártová, H.; Trojek, T.; Johnová, K.

2017-11-01

This article describes the method for the estimation of depth distribution of radionuclides in a material with gamma-ray spectrometry, and the identification of a layered structure of a material with X-ray fluorescence analysis. This method is based on the measurement of a ratio of two gamma or X-ray lines of a radionuclide or a chemical element, respectively. Its principle consists in different attenuation coefficient for these two lines in a measured material. The main aim of this investigation was to show how the detected ratio of these two lines depends on depth distribution of an analyte and mainly how this ratio depends on density and chemical composition of measured materials. Several different calculation arrangements were made and a lot of Monte Carlo simulation with the code MCNP - Monte Carlo N-Particle (Briesmeister, 2000) was performed to answer these questions. For X-ray spectrometry, the calculated Kα/Kβ diagrams were found to be almost independent upon matrix density and composition. Thanks to this phenomenon it would be possible to draw only one Kα/Kβ diagram for an element whose depth distribution is examined.

SSRL HEADLINES April 2018

Science.gov Websites

and x-ray spectroscopy pioneer, Farrel W. Lytle, and include precious metals such as gold, silver structure of matter called x-ray absorption spectroscopy. The foils were donated by entrepreneur, scientist activities on x-ray fluorescence imaging in ancient materials like fossils and the Archimedes Palimpsest

Bio-metals imaging and speciation in cells using proton and synchrotron radiation X-ray microspectroscopy

PubMed Central

Ortega, Richard; Devès, Guillaume; Carmona, Asunción

2009-01-01

The direct detection of biologically relevant metals in single cells and of their speciation is a challenging task that requires sophisticated analytical developments. The aim of this article is to present the recent achievements in the field of cellular chemical element imaging, and direct speciation analysis, using proton and synchrotron radiation X-ray micro- and nano-analysis. The recent improvements in focusing optics for MeV-accelerated particles and keV X-rays allow application to chemical element analysis in subcellular compartments. The imaging and quantification of trace elements in single cells can be obtained using particle-induced X-ray emission (PIXE). The combination of PIXE with backscattering spectrometry and scanning transmission ion microscopy provides a high accuracy in elemental quantification of cellular organelles. On the other hand, synchrotron radiation X-ray fluorescence provides chemical element imaging with less than 100 nm spatial resolution. Moreover, synchrotron radiation offers the unique capability of spatially resolved chemical speciation using micro-X-ray absorption spectroscopy. The potential of these methods in biomedical investigations will be illustrated with examples of application in the fields of cellular toxicology, and pharmacology, bio-metals and metal-based nano-particles. PMID:19605403

Soft X-ray spectromicroscopy for speciation, quantitation and nano-eco-toxicology of nanomaterials.

PubMed

Lawrence, J R; Swerhone, G D W; Dynes, J J; Korber, D R; Hitchcock, A P

2016-02-01

There is a critical need for methods that provide simultaneous detection, identification, quantitation and visualization of nanomaterials at their interface with biological and environmental systems. The approach should allow speciation as well as elemental analysis. Using the intrinsic X-ray absorption properties, soft X-ray scanning transmission X-ray spectromicroscopy (STXM) allows characterization and imaging of a broad range of nanomaterials, including metals, oxides and organic materials, and at the same time is able to provide detailed mapping of biological components. Thus, STXM offers considerable potential for application to research on nanomaterials in biology and the environment. The potential and limitations of STXM in this context are discussed using a range of examples, focusing on the interaction of nanomaterials with microbial cells, biofilms and extracellular polymers. The studies outlined include speciation and mapping of metal-containing nanomaterials (Ti, Ni, Cu) and carbon-based nanomaterials (multiwalled carbon nanotubes, C60 fullerene). The benefits of X-ray fluorescence detection in soft X-ray STXM are illustrated with a study of low levels of Ni in a natural river biofilm. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

Transmission X-ray microscopy for full-field nano-imaging of biomaterials

PubMed Central

ANDREWS, JOY C; MEIRER, FLORIAN; LIU, YIJIN; MESTER, ZOLTAN; PIANETTA, PIERO

2010-01-01

Imaging of cellular structure and extended tissue in biological materials requires nanometer resolution and good sample penetration, which can be provided by current full-field transmission X-ray microscopic techniques in the soft and hard X-ray regions. The various capabilities of full-field transmission X-ray microscopy (TXM) include 3D tomography, Zernike phase contrast, quantification of absorption, and chemical identification via X-ray fluorescence and X-ray absorption near edge structure (XANES) imaging. These techniques are discussed and compared in light of results from imaging of biological materials including microorganisms, bone and mineralized tissue and plants, with a focus on hard X-ray TXM at ≤ 40 nm resolution. PMID:20734414

[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.

Abundance and Charge State of Implanted Solar Wind Transition Metals in Individual Apollo 16 and 17 Lunar Soil Plagioclase Grains Determined In Situ Using Synchrotron X-ray Fluorescence

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

Kitts, K.; Sutton, S.; Newville, M.

2007-03-06

We report (1) a new method for determining the relative abundances in situ of Cr, Mn, Fe and Ni in implanted solar wind in individual Apollo 16 and 17 lunar plagioclases via synchrotron X-ray fluorescence and (2) the charge states of these metals. By virture of its mass alone, the Sun provides a representative composition of the solar system and can be used as a background against which to gauge excesses or deficiencies of specific components. One way of sampling the Sun is by measuring solar wind implanted ions in lunar soil grains. Such measurements are valuable because of theirmore » long exposure ages which compliment shorter time scale collections, such as those obtained by the Genesis spacecraft. Kitts et al. sought to determine the isotopic composition of solar Cr by analyzing the solar wind implanted into plagioclase grains from Apollo 16 lunar soils. The isotopic composition of the solar wind bearing fraction was anomalous and did not match any other known Cr isotopic signature. This could only be explained by either (1) an enrichment in the solar wind of heavy Cr due to spallation in the solar atmosphere or (2) that the Earth and the various parent bodies of the meteorites are distinct from the Sun and must have formed from slightly different mixes of presolar materials. To help resolve this issue, we have developed a wholly independent method for determining the relative abundances of transition metals in the solar wind implanted in individual lunar soil grains. This method is based on in situ abundance measurements by microbeam x-ray fluorescence in both the implantation zone and bulk grains using the synchrotron x-ray microprobe at the Advanced Photon Source (GSECARS sector 13) at Argonne National Laboratory. Here, we report results for Apollo 16 and 17 plagioclase grains. Additionally, a micro-XANES technique was used to determine charge states of the implanted Cr, Mn, Fe and Ni.« less

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.

Observation and analysis of microcirculation using high-spatial-resolution image detectors and synchrotron radiation

NASA Astrophysics Data System (ADS)

Umetani, Keiji; Yagi, Naoto; Suzuki, Yoshio; Ogasawara, Yasuo; Kajiya, Fumihiko; Matsumoto, Takeshi; Tachibana, Hiroyuki; Goto, Masami; Yamashita, Takenori; Imai, Shigeki; Kajihara, Yasumasa

2000-04-01

A microangiography system using monochromatized synchrotron radiation has been investigated as a diagnostic tool for circulatory disorders and early stage malignant tumors. The monochromatized X-rays with energies just above the contrast agent K-absorption edge energy can produce the highest contrast image of the contrast agent in small blood vessels. At SPring-8, digital microradiography with 6 - 24 micrometer pixel sizes has been carried out using two types of detectors designed for X-ray indirect and direct detection. The indirect-sensing detectors are fluorescent-screen optical-lens coupling systems using a high-sensitivity pickup-tube camera and a CCD camera. An X-ray image on the fluorescent screen is focused on the photoconductive layer of the pickup tube and the photosensitive area of the CCD by a small F number lens. The direct-sensing detector consists of an X-ray direct- sensing pickup tube with a beryllium faceplate for X-ray incidence to the photoconductive layer. Absorbed X-rays in the photoconductive layer are directly converted to photoelectrons and then signal charges are readout by electron beam scanning. The direct-sensing detector was expected to have higher spatial resolution in comparison with the indict-sensing detectors. Performance of the X-ray image detectors was examined at the bending magnet beamline BL20B2 using monochromatized X-ray at SPring-8. Image signals from the camera are converted into digital format by an analog-to- digital converter and stored in a frame memory with image format of 1024 X 1024 pixels. In preliminary experiments, tumor vessel specimens using barium contrast agent were prepared for taking static images. The growth pattern of tumor-induced vessels was clearly visualized. Heart muscle specimens were prepared for imaging of 3-dimensional microtomography using the fluorescent-screen CCD camera system. The complex structure of small blood vessels with diameters of 30 - 40 micrometer was visualized as a 3- dimensional CT image.

Intracellular in situ labeling of TiO2 nanoparticles for fluorescence microscopy detection

PubMed Central

Brown, Koshonna; Thurn, Ted; Xin, Lun; Liu, William; Bazak, Remon; Chen, Si; Lai, Barry; Vogt, Stefan; Jacobsen, Chris; Paunesku, Tatjana; Woloschak, Gayle E.

2018-01-01

Titanium dioxide (TiO2) nanoparticles are produced for many different purposes, including development of therapeutic and diagnostic nanoparticles for cancer detection and treatment, drug delivery, induction of DNA double-strand breaks, and imaging of specific cells and subcellular structures. Currently, the use of optical microscopy, an imaging technique most accessible to biology and medical pathology, to detect TiO2 nanoparticles in cells and tissues ex vivo is limited with low detection limits, while more sensitive imaging methods (transmission electron microscopy, X-ray fluorescence microscopy, etc.) have low throughput and technical and operational complications. Herein, we describe two in situ post-treatment labeling approaches to stain TiO2 nanoparticles taken up by the cells. The first approach utilizes fluorescent biotin and fluorescent streptavidin to label the nanoparticles before and after cellular uptake; the second approach is based on the copper-catalyzed azide-alkyne cycloaddition, the so-called Click chemistry, for labeling and detection of azide-conjugated TiO2 nanoparticles with alkyne-conjugated fluorescent dyes such as Alexa Fluor 488. To confirm that optical fluorescence signals of these nanoparticles match the distribution of the Ti element, we used synchrotron X-ray fluorescence microscopy (XFM) at the Advanced Photon Source at Argonne National Laboratory. Titanium-specific XFM showed excellent overlap with the location of optical fluorescence detected by confocal microscopy. Therefore, future experiments with TiO2 nanoparticles may safely rely on confocal microscopy after in situ nanoparticle labeling using approaches described here. PMID:29541425

Intracellular in situ labeling of TiO2 nanoparticles for fluorescence microscopy detection.

PubMed

Brown, Koshonna; Thurn, Ted; Xin, Lun; Liu, William; Bazak, Remon; Chen, Si; Lai, Barry; Vogt, Stefan; Jacobsen, Chris; Paunesku, Tatjana; Woloschak, Gayle E

2018-01-01

Titanium dioxide (TiO 2 ) nanoparticles are produced for many different purposes, including development of therapeutic and diagnostic nanoparticles for cancer detection and treatment, drug delivery, induction of DNA double-strand breaks, and imaging of specific cells and subcellular structures. Currently, the use of optical microscopy, an imaging technique most accessible to biology and medical pathology, to detect TiO 2 nanoparticles in cells and tissues ex vivo is limited with low detection limits, while more sensitive imaging methods (transmission electron microscopy, X-ray fluorescence microscopy, etc.) have low throughput and technical and operational complications. Herein, we describe two in situ post-treatment labeling approaches to stain TiO 2 nanoparticles taken up by the cells. The first approach utilizes fluorescent biotin and fluorescent streptavidin to label the nanoparticles before and after cellular uptake; the second approach is based on the copper-catalyzed azide-alkyne cycloaddition, the so-called Click chemistry, for labeling and detection of azide-conjugated TiO 2 nanoparticles with alkyne-conjugated fluorescent dyes such as Alexa Fluor 488. To confirm that optical fluorescence signals of these nanoparticles match the distribution of the Ti element, we used synchrotron X-ray fluorescence microscopy (XFM) at the Advanced Photon Source at Argonne National Laboratory. Titanium-specific XFM showed excellent overlap with the location of optical fluorescence detected by confocal microscopy. Therefore, future experiments with TiO 2 nanoparticles may safely rely on confocal microscopy after in situ nanoparticle labeling using approaches described here.

The effect of X-ray exposure on Ba2SiO4:Eu3+

NASA Astrophysics Data System (ADS)

Volhard, Max-Fabian; Jüstel, Thomas

2018-03-01

The ortho-silicates Ba2SiO4:Eu3+ and Ba2SiO4:Eu2+ are well-established materials for fluorescent light sources, e.g., phosphor converted LEDs. Samples containing Eu2+or Eu3+were synthesised by the solid-state-method, and the phase purity was determined by X-ray powder diffractometry. The photoluminescence of both phosphors was examined as a function of the pre-treatment. Upon irradiation of Ba2SiO4:Eu3+ with X-rays (tungsten target source), the reduction of Eu3+ towards Eu2+ was observed. This reduction behaviour was thoroughly recorded, and the linearity of the process was determined. Furthermore, the relationship between the acceleration voltage and the reduction process is discussed.

Self-consistent method for quantifying indium content from X-ray spectra of thick compound semiconductor specimens in a transmission electron microscope.

PubMed

Walther, T; Wang, X

2016-05-01

Based on Monte Carlo simulations of X-ray generation by fast electrons we calculate curves of effective sensitivity factors for analytical transmission electron microscopy based energy-dispersive X-ray spectroscopy including absorption and fluorescence effects, as a function of Ga K/L ratio for different indium and gallium containing compound semiconductors. For the case of InGaN alloy thin films we show that experimental spectra can thus be quantified without the need to measure specimen thickness or density, yielding self-consistent values for quantification with Ga K and Ga L lines. The effect of uncertainties in the detector efficiency are also shown to be reduced. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Archimedes and the Golden Crown

ERIC Educational Resources Information Center

Thompson, Frank

2008-01-01

Archimedes (287-212 BC) is well known for his explanation of buoyancy, and in particular for his "eureka" moment. This experiment uses his density measurement method to find the purity of gold, and additional confirmation of the findings are given by x-ray fluorescence. (Contains 4 figures and 1 table.)

X-ray fluorescence spectrometry-based approach to precision management of bioavailable phosphorus in soil environments

USDA-ARS?s Scientific Manuscript database

Declining nutrient use efficiency in crop production has been a global priority to preserve high agricultural productivity with finite non-renewable nutrient resources, in particular phosphorus (P). Rapid spectroscopic methods increase measurement density of soil nutrients, and the availability of ...

Quantitative X-ray diffraction and fluorescence analysis of paint pigment systems : final report.

DOT National Transportation Integrated Search

1978-01-01

This study attempted to correlate measured X-ray intensities with concentrations of each member of paint pigment systems, thereby establishing calibration curves for the quantitative analyses of such systems.

Halide Ions Effects on Surface Excess of Long Chain Ionic Liquids Water Solutions

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

Wang, Wenjie; Sung, Woongmo; Ao, Mingqi

2013-10-07

The interfacial structure and composition of water solutions with alkylimidazolium ionic liquids varying in their halide anions ([C12mim][X], X = Cl and I) were investigated by X-ray near-total-reflection fluorescence spectroscopy and X-ray reflectivity measurements. We demonstrate that X-ray fluorescence and reflectivity techniques provide a more direct measurement of surface adsorption. Furthermore, we show that for [C12mim][Cl] and [C12mim][I] solutions with mixed inorganic salts (NaI, NaCl), I– ions replace Cl– above the critical micelle concentration (CMC) of [C12mim][Cl] at much lower concentrations of NaI, whereas NaCl concentrations a hundred times higher than the CMC of [C12mim][I] only partially replace the I–more » at the interface. Our surface-sensitive X-ray diffraction and spectroscopy provide two independent tools to directly determine the surface adsorption of ionic surfactants and the interfacial composition of the surface films.« less

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

NASA Astrophysics Data System (ADS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-10-01

Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV-vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

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

Characterization of the external and internal flow structure of an aerated-liquid injector using X-ray radiography and fluorescence

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

Peltier, Scott J.; Lin, Kuo-Cheng; Carter, Campbell D.

In the present study, the internal flowfield of aerated-liquid fuel injectors is examined through x-ray radiography and x-ray fluorescence. An inside-out injector, consisting of a perforated aerating tube within an annular liquid stream, sprays into a quiescent environment at a fixed mass flow rate of water and nitrogen gas. The liquid is doped with bromine (in the form of NaBr) to create an x-ray fluorescence signal. This allows for reasonable absorption and fluorescence signals, and one or both diagnostics can be used to track the liquid distribution. The injector housing is fabricated from beryllium (Be), which allows the internal flowfieldmore » to be examined (as Be has relatively low x-ray attenuation coefficient). Two injector geometries are compared, illustrating the effects of aerating orifice size and location on the flow evolution. Time-averaged equivalent pathlength (EPL) and line-of-sight averaged density ρ(y) reveal the formation of the two-phase mixture, showing that the liquid film thickness along the injector walls is a function of the aerating tube geometry, though only upstream of the nozzle. These differences in gas and liquid distribution (between injectors with different aerating tube designs) are suppressed as the mixture traverses the nozzle contraction. The averaged liquid velocity (computed from the density and liquid mass flow rate) reveal a similar trend. This suggests that at least for the current configurations, the plume width, liquid mass distribution, and averaged liquid velocity for the time-averaged external spray are insensitive to the aerating tube geometry.« less

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.

Mass attenuation coefficients in the range 3.8⩽E⩽11 keV, K fluorescence yield and Kβ/Kα relative X-ray emission rate for Ti, V, Fe, Co, Ni, Cu and Zn measured with a tunable monochromatic X-ray source

NASA Astrophysics Data System (ADS)

Ménesguen, Y.; Lépy, M.-C.

2010-08-01

This work presents new measurements of mass attenuation coefficients in the range 3.8⩽E⩽11 keV, K-absorption jump-ratios, Kα and Kβ fluorescence yields for Ti, V, Fe, Co, Ni, Cu and Zn. We use the experimental facility SOLEX, a tunable monochromatic X-ray source combined with an energy-dispersive high-purity germanium detector. The results are compared with theoretical values as well as with other experimental data and show a relatively good agreement. However, the derived K-jump-ratios appear larger than those widely used in the XCOM database. The Kα and Kβ fluorescence yields and the corresponding relative emission rates Kβ/Kα are also derived, which was made possible by the use of energy-dispersive detectors with good spectral resolution.

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-induced fluorescent centers formation in zinc- phosphate glasses doped with Ag and Cu ions

NASA Astrophysics Data System (ADS)

Klyukin, D. A.; Pshenova, A. S.; Sidorov, A. I.; Stolyarchuk, M. V.

2016-08-01

Fluorescent properties of silver and copper doped zinc-phosphate glasses were studied. By X-ray irradiation of silver and copper co-doped glasses we could create and identify new emission centers which do not exist in single-doped samples. Doping of the glass with both silver and copper ions leads to the increase of quantum yield by 2.7 times. The study was complemented by quantum chemical calculations using the time-dependent density functional theory. It was shown that fluorescence may be attributed to the formation of mixed Ag-Cu molecular clusters.

Synthesis, microstructure, and magnetic properties of monosized Mn x Zn y Fe3 − x − y O4 ferrite nanocrystals

PubMed Central

2013-01-01

We report the synthesis and characterization of ferrite nanocrystals which exhibit high crystallinity and narrow size distributions. The three types of samples including Zn ferrite, Mn ferrite, and Mn-Zn ferrite were prepared via a non-aqueous nanoemulsion method. The structural, chemical, and magnetic properties of the nanocrystals are analyzed by transmission electron microscopy, X-ray diffraction, X-ray fluorescence, and physical property measurement system. The characterization indicates that the three types of ferrite nanocrystals were successfully produced, which show well-behaved magnetic properties, ferrimagnetism at 5 K and superparamagnetism at 300 K, respectively. In addition, the magnetization value of the ferrites increases with the increasing concentration of Mn. PMID:24344630

Theoretical and experimental determination of K - and L -shell x-ray relaxation parameters in Ni

NASA Astrophysics Data System (ADS)

Guerra, M.; Sampaio, J. M.; Parente, F.; Indelicato, P.; Hönicke, P.; Müller, M.; Beckhoff, B.; Marques, J. P.; Santos, J. P.

2018-04-01

Fluorescence yields (FY) for the Ni K and L shells were determined by a theoretical and an experimental group within the framework of the International Initiative on X-ray Fundamental Parameters (FPs) collaboration. Coster-Kronig (CK) parameters were also measured for the L shell of Ni. Theoretical calculations of the same parameters were performed using the Dirac-Fock method, including relativistic and QED corrections. The experimental values for the FY and CK were determined at the PTB laboratory in the synchrotron radiation facility BESSY II, Berlin, Germany, and are compared to the corresponding calculated values.

The effect of ultrasonic irradiation on the crystallinity of nano-hydroxyapatite produced via the wet chemical method.

PubMed

Barbosa, Michelle C; Messmer, Nigel R; Brazil, Tayra R; Marciano, Fernanda R; Lobo, Anderson O

2013-07-01

Nanohydroxyapatite (nHAp) powders were produced via aqueous precipitation by adopting four different experimental conditions, assisted or non-assisted by ultrasound irradiation (UI). The nHAp powders were characterized by X-ray diffraction, energy-dispersive X-ray fluorescence, Raman and attenuated total reflection Fourier transform infrared spectroscopies, which showed typical surface chemical compositions of nHAp. Analysis found strong connections between UI and the crystallization process, crystal growth properties, as well as correlations between calcination and substitution reactions. Copyright © 2013 Elsevier B.V. All rights reserved.

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

Manohar, N; Cho, S; Reynoso, F

Purpose: To make benchtop x-ray fluorescence computed tomography (XFCT) practical for routine preclinical imaging tasks with gold nanoparticles (GNPs) by deploying, integrating, and characterizing a dedicated high-performance x-ray source and addition of simultaneous micro-CT functionality. Methods: Considerable research effort is currently under way to develop a polychromatic benchtop cone-beam XFCT system capable of imaging GNPs by stimulation and detection of gold K-shell x-ray fluorescence (XRF) photons. Recently, an ad hoc high-power x-ray source was incorporated and used to image the biodistribution of GNPs within a mouse, postmortem. In the current work, a dedicated x-ray source system featuring a liquid-cooled tungsten-targetmore » x-ray tube (max 160 kVp, ∼3 kW power) was deployed. The source was operated at 125 kVp, 24 mA. The tube’s compact dimensions allowed greater flexibility for optimizing both the irradiation and detection geometries. Incident x-rays were shaped by a conical collimator and filtered by 2 mm of tin. A compact “OEM” cadmium-telluride x-ray detector was implemented for detecting XRF/scatter spectra. Additionally, a flat panel detector was installed to allow simultaneous transmission CT imaging. The performance of the system was characterized by determining the detection limit (10-second acquisition time) for inserts filled with water/GNPs at various concentrations (0 and 0.010–1.0 wt%) and embedded in a small-animal-sized phantom. The phantom was loaded with 0.5, 0.3, and 0.1 wt% inserts and imaged using XFCT and simultaneous micro-CT. Results: An unprecedented detection limit of 0.030 wt% was experimentally demonstrated, with a 33% reduction in acquisition time. The reconstructed XFCT image accurately localized the imaging inserts. Micro-CT imaging did not provide enough contrast to distinguish imaging inserts from the phantom under the current conditions. Conclusion: The system is immediately capable of in vivo preclinical XFCT imaging with GNPs. Micro-CT imaging will require optimization of irradiation parameters to improve contrast. Supported by NIH/NCI grant R01CA155446; This investigation was supported by NIH/NCI grant R01CA155446.« less

A new spectrometer for total reflection X-ray fluorescence analysis of light elements

NASA Astrophysics Data System (ADS)

Streli, Christina; Wobrauschek, Peter; Unfried, Ernst; Aiginger, Hannes

1993-10-01

A new spectrometer for total reflection X-ray fluorescence analysis (TXRF) of light elements as C, N, O, F, Na,… has been designed, constructed and realized. This was done under the aspect of optimizing all relevant parameters for excitation and detection under the conditions of Total Reflection in a vacuum chamber. A commercially available Ge(HP) detector with a diamond window offering a high transparency for low energy radiation was used. As excitation sources a special self-made windowless X-ray tube with Cu-target as well as a standard fine-focus Cr-tube were applied. Detection limits achieved are in the ng range for Carbon and Oxygen.

Fast automatic segmentation of anatomical structures in x-ray computed tomography images to improve fluorescence molecular tomography reconstruction.

PubMed

Freyer, Marcus; Ale, Angelique; Schulz, Ralf B; Zientkowska, Marta; Ntziachristos, Vasilis; Englmeier, Karl-Hans

2010-01-01

The recent development of hybrid imaging scanners that integrate fluorescence molecular tomography (FMT) and x-ray computed tomography (XCT) allows the utilization of x-ray information as image priors for improving optical tomography reconstruction. To fully capitalize on this capacity, we consider a framework for the automatic and fast detection of different anatomic structures in murine XCT images. To accurately differentiate between different structures such as bone, lung, and heart, a combination of image processing steps including thresholding, seed growing, and signal detection are found to offer optimal segmentation performance. The algorithm and its utilization in an inverse FMT scheme that uses priors is demonstrated on mouse images.

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.

Structural and elemental changes in glioblastoma cells in situ: complementary imaging with high resolution visible light- and X-ray microscopy

DOE PAGES

Ducic, Tanja; Paunesku, Tatjana; Chen, Si; ...

2016-12-09

The glioblastoma (GBM) is characterized by a short median survival and an almost 100% tumor related mortality. GBM cells exhibit highly invasive behavior whose mechanisms are not yet fully understood. The present study explores application of X-ray and visible light microscopy to display the elemental and structural images of cells from 3 patient derived GMB samples and an established GMB cell line. Slight differences in elemental concentrations, in actin cytoskeleton organization and cell morphology were noted between all cells types by X-ray fluorescence and full field soft X-ray microscopy, as well as the Structured Illumination Super-resolution Microscope (SIM). Different samplemore » preparation approaches were used to match each imaging technique. While preparation for SIM included cell fixation and staining, intact frozen hydrated cells were used for the trace element imaging by hard X-ray fluorescence and exploration of the structural features by soft X-ray absorption tomography. In conclusion, each technique documented differences between samples with regard to morphology and elemental composition and underscored the importance of use of multiple patient derived samples for detailed GBM study.« 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.

Structural and elemental changes in glioblastoma cells in situ: complementary imaging with high resolution visible light- and X-ray microscopy

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

Ducic, Tanja; Paunesku, Tatjana; Chen, Si

The glioblastoma (GBM) is characterized by a short median survival and an almost 100% tumor related mortality. GBM cells exhibit highly invasive behavior whose mechanisms are not yet fully understood. The present study explores application of X-ray and visible light microscopy to display the elemental and structural images of cells from 3 patient derived GMB samples and an established GMB cell line. Slight differences in elemental concentrations, in actin cytoskeleton organization and cell morphology were noted between all cells types by X-ray fluorescence and full field soft X-ray microscopy, as well as the Structured Illumination Super-resolution Microscope (SIM). Different samplemore » preparation approaches were used to match each imaging technique. While preparation for SIM included cell fixation and staining, intact frozen hydrated cells were used for the trace element imaging by hard X-ray fluorescence and exploration of the structural features by soft X-ray absorption tomography. In conclusion, each technique documented differences between samples with regard to morphology and elemental composition and underscored the importance of use of multiple patient derived samples for detailed GBM study.« less

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

NASA Technical Reports Server (NTRS)

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

1999-01-01

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

Analytical Energy Dispersive X-Ray Fluorescence Measurements with a Scanty Amounts of Plant and Soil Materials

NASA Astrophysics Data System (ADS)

Mittal, R.; Rao, P.; Kaur, P.

2018-01-01

Elemental evaluations in scanty powdered material have been made using energy dispersive X-ray fluorescence (EDXRF) measurements, for which formulations along with specific procedure for sample target preparation have been developed. Fractional amount evaluation involves an itinerary of steps; (i) collection of elemental characteristic X-ray counts in EDXRF spectra recorded with different weights of material, (ii) search for linearity between X-ray counts and material weights, (iii) calculation of elemental fractions from the linear fit, and (iv) again linear fitting of calculated fractions with sample weights and its extrapolation to zero weight. Thus, elemental fractions at zero weight are free from material self absorption effects for incident and emitted photons. The analytical procedure after its verification with known synthetic samples of macro-nutrients, potassium and calcium, was used for wheat plant/ soil samples obtained from a pot experiment.

Observation of divergent-beam X-ray diffraction from a crystal of diamond using synchrotron radiation.

PubMed

Glazer, A M; Collins, S P; Zekria, D; Liu, J; Golshan, M

2004-03-01

In 1947 Kathleen Lonsdale conducted a series of experiments on X-ray diffraction using a divergent beam external to a crystal sample. Unlike the Kossel technique, where divergent X-rays are excited by the presence of fluorescing atoms within the crystal, the use of an external divergent source made it possible to study non-fluorescing crystals. The resulting photographs not only illustrated the complexity of X-ray diffraction from crystals in a truly beautiful way, but also demonstrated unprecedented experimental precision. This long-forgotten work is repeated here using a synchrotron radiation source and, once again, considerable merit is found in Lonsdale's technique. The results of this experiment suggest that, through the use of modern 'third-generation' synchrotron sources, divergent-beam diffraction could soon enjoy a renaissance for high-precision lattice-parameter determination and the study of crystal perfection.

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.

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.

Quantitative Electron Probe Microanalysis: State of the Art

NASA Technical Reports Server (NTRS)

Carpernter, P. K.

2005-01-01

Quantitative electron-probe microanalysis (EPMA) has improved due to better instrument design and X-ray correction methods. Design improvement of the electron column and X-ray spectrometer has resulted in measurement precision that exceeds analytical accuracy. Wavelength-dispersive spectrometer (WDS) have layered-dispersive diffraction crystals with improved light-element sensitivity. Newer energy-dispersive spectrometers (EDS) have Si-drift detector elements, thin window designs, and digital processing electronics with X-ray throughput approaching that of WDS Systems. Using these systems, digital X-ray mapping coupled with spectrum imaging is a powerful compositional mapping tool. Improvements in analytical accuracy are due to better X-ray correction algorithms, mass absorption coefficient data sets,and analysis method for complex geometries. ZAF algorithms have ban superceded by Phi(pz) algorithms that better model the depth distribution of primary X-ray production. Complex thin film and particle geometries are treated using Phi(pz) algorithms, end results agree well with Monte Carlo simulations. For geological materials, X-ray absorption dominates the corretions end depends on the accuracy of mass absorption coefficient (MAC) data sets. However, few MACs have been experimentally measured, and the use of fitted coefficients continues due to general success of the analytical technique. A polynomial formulation of the Bence-Albec alpha-factor technique, calibrated using Phi(pz) algorithms, is used to critically evaluate accuracy issues and can be also be used for high 2% relative and is limited by measurement precision for ideal cases, but for many elements the analytical accuracy is unproven. The EPMA technique has improved to the point where it is frequently used instead of the petrogaphic microscope for reconnaissance work. Examples of stagnant research areas are: WDS detector design characterization of calibration standards, and the need for more complete treatment of the continuum X-ray fluorescence correction.

Efficient Simulation of Secondary Fluorescence Via NIST DTSA-II Monte Carlo.

PubMed

Ritchie, Nicholas W M

2017-06-01

Secondary fluorescence, the final term in the familiar matrix correction triumvirate Z·A·F, is the most challenging for Monte Carlo models to simulate. In fact, only two implementations of Monte Carlo models commonly used to simulate electron probe X-ray spectra can calculate secondary fluorescence-PENEPMA and NIST DTSA-II a (DTSA-II is discussed herein). These two models share many physical models but there are some important differences in the way each implements X-ray emission including secondary fluorescence. PENEPMA is based on PENELOPE, a general purpose software package for simulation of both relativistic and subrelativistic electron/positron interactions with matter. On the other hand, NIST DTSA-II was designed exclusively for simulation of X-ray spectra generated by subrelativistic electrons. NIST DTSA-II uses variance reduction techniques unsuited to general purpose code. These optimizations help NIST DTSA-II to be orders of magnitude more computationally efficient while retaining detector position sensitivity. Simulations execute in minutes rather than hours and can model differences that result from detector position. Both PENEPMA and NIST DTSA-II are capable of handling complex sample geometries and we will demonstrate that both are of similar accuracy when modeling experimental secondary fluorescence data from the literature.

Characterization of pigments and colors used in ancient Egyptian boat models

NASA Astrophysics Data System (ADS)

Hühnerfuβ, Katja; von Bohlen, Alex; Kurth, Dieter

2006-11-01

The analyses of pigments originating from well dated ancient boat models found in Egyptian graves were used for characterization and for dating tasks of unknown objects. A nearly destruction free sampling technique using cotton buds was applied for sampling these valuable artifacts for a subsequent Total Reflection X-Ray Fluorescence Spectrometry (TXRF) analysis. Two relevant collections of Egyptian object of art were at our disposal, one of the Ägyptisches Museum Berlin and the second of the British Museum London. Three groups of colors were studied, they originate from white, red and blue/green paints, respectively. The results of the analyses performed on micro-amounts of paints (< 1 μg) show that some artifacts were misclassified and belong to other epochs. Some others were retouched with modern colors. In general, it can be stated that results obtained by Total Reflection X-Ray Fluorescence Spectrometry may dissipate some uncertainties when applying classical archaeological dating methods.

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.

X-ray fluorescence analysis of K, Al and trace elements in chloroaluminate melts

NASA Astrophysics Data System (ADS)

Shibitko, A. O.; Abramov, A. V.; Denisov, E. I.; Lisienko, D. G.; Rebrin, O. I.; Bunkov, G. M.; Rychkov, V. N.

2017-09-01

Energy dispersive x-ray fluorescence spectrometry was applied to quantitative determination of K, Al, Cr, Fe and Ni in chloroaluminate melts. To implement the external standard calibration method, an unconventional way of samples preparation was suggested. A mixture of metal chlorides was melted in a quartz cell at 350-450 °C under a slightly excessive pressure of purified argon (99.999 %). The composition of the calibration samples (CSs) prepared was controlled by means of the inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimal conditions for analytical lines excitation were determined, the analytes calibration curves were obtained. There was some influence of matrix effects in synthesized samples on the analytical signal of some elements. The CSs are to be stored in inert gas atmosphere. The precision, accuracy, and reproducibility factors of the quantitative chemical analysis were computed.

The characterization of canvas painting by the Serbian artist Milo Milunović using X-ray fluorescence, micro-Raman and FTIR spectroscopy

NASA Astrophysics Data System (ADS)

Damjanović, Lj.; Gajić-Kvaščev, M.; Đurđević, J.; Andrić, V.; Marić-Stojanović, M.; Lazić, T.; Nikolić, S.

2015-10-01

A canvas painting by Milo Milunović "The Inspiration of the poet" was studied by energy dispersive X-Ray fluorescence (EDXRF), micro-Raman and Fourier transform infrared (FTIR) spectroscopy in order to identify materials used by the artist and his painting technique. Study is perfomed combining in situ non-destructive method with the preparation and study of cross-section samples and raw fragments of the samples. Milo Milunović, an eminent painter from Balkan region, made a copy of the Nicolas Poussin's original painting in Louvre in 1926/27. Obtained results revealed following pigments on the investigated canvas painting: vermilion, minium, cobalt blue, ultramarine, lead white, zinc white, cadmium yellow, chrome-based green pigment and several earth pigments - red and yellow ocher, green earth and umber. Ground layer was made of lead white mixed with calcium carbonate.

Hyperspectral image reconstruction for x-ray fluorescence tomography

DOE PAGES

Gürsoy, Doǧa; Biçer, Tekin; Lanzirotti, Antonio; ...

2015-01-01

A penalized maximum-likelihood estimation is proposed to perform hyperspectral (spatio-spectral) image reconstruction for X-ray fluorescence tomography. The approach minimizes a Poisson-based negative log-likelihood of the observed photon counts, and uses a penalty term that has the effect of encouraging local continuity of model parameter estimates in both spatial and spectral dimensions simultaneously. The performance of the reconstruction method is demonstrated with experimental data acquired from a seed of arabidopsis thaliana collected at the 13-ID-E microprobe beamline at the Advanced Photon Source. The resulting element distribution estimates with the proposed approach show significantly better reconstruction quality than the conventional analytical inversionmore » approaches, and allows for a high data compression factor which can reduce data acquisition times remarkably. In particular, this technique provides the capability to tomographically reconstruct full energy dispersive spectra without compromising reconstruction artifacts that impact the interpretation of results.« less

Semi-quantitative estimation of cellular SiO2 nanoparticles using flow cytometry combined with X-ray fluorescence measurements.

PubMed

Choi, Seo Yeon; Yang, Nuri; Jeon, Soo Kyung; Yoon, Tae Hyun

2014-09-01

In this study, we have demonstrated feasibility of a semi-quantitative approach for the estimation of cellular SiO2 nanoparticles (NPs), which is based on the flow cytometry measurements of their normalized side scattering intensity. In order to improve our understanding on the quantitative aspects of cell-nanoparticle interactions, flow cytometry, transmission electron microscopy, and X-ray fluorescence experiments were carefully performed for the HeLa cells exposed to SiO2 NPs with different core diameters, hydrodynamic sizes, and surface charges. Based on the observed relationships among the experimental data, a semi-quantitative cellular SiO2 NPs estimation method from their normalized side scattering and core diameters was proposed, which can be applied for the determination of cellular SiO2 NPs within their size-dependent linear ranges. © 2014 International Society for Advancement of Cytometry.

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.

Transmission X-ray microscopy for full-field nano imaging of biomaterials.

PubMed

Andrews, Joy C; Meirer, Florian; Liu, Yijin; Mester, Zoltan; Pianetta, Piero

2011-07-01

Imaging of cellular structure and extended tissue in biological materials requires nanometer resolution and good sample penetration, which can be provided by current full-field transmission X-ray microscopic techniques in the soft and hard X-ray regions. The various capabilities of full-field transmission X-ray microscopy (TXM) include 3D tomography, Zernike phase contrast, quantification of absorption, and chemical identification via X-ray fluorescence and X-ray absorption near edge structure imaging. These techniques are discussed and compared in light of results from the imaging of biological materials including microorganisms, bone and mineralized tissue, and plants, with a focus on hard X-ray TXM at ≤ 40-nm resolution. Copyright © 2010 Wiley-Liss, Inc.

40 CFR 1065.1010 - Incorporation by reference.

Code of Federal Regulations, 2014 CFR

2014-07-01

... approved for § 1065.701(f). (43) ASTM D6751-12, Standard Specification for Biodiesel Fuel Blend Stock (B100... D7039-13, Standard Test Method for Sulfur in Gasoline, Diesel Fuel, Jet Fuel, Kerosine, Biodiesel, Biodiesel Blends, and Gasoline-Ethanol Blends by Monochromatic Wavelength Dispersive X-ray Fluorescence...

Determination of selenium in the environment and in biological material.

PubMed Central

Bem, E M

1981-01-01

This paper reviews the following problems, sampling, decomposition procedures and most important analytical methods used for selenium determination, e.g., neutron activation analysis, atomic absorption spectrometry, gas-liquid chromatography, spectrophotometry, fluorimetry, and x-ray fluorescence. This review covers the literature mainly from 1975 to 1977. PMID:7007035

X-ray based displacement and strain measurements for hostile environments

NASA Technical Reports Server (NTRS)

Canistraro, Howard A.; Jordan, Eric H.; Pease, Douglas M.

1993-01-01

A completely new method of non-contacting, hostile environment displacement and strain measurement based on the focus and scanning of x-rays, has been developed and demonstrated. The new technique has the ability to overcome many of the limitations associated with available methods. The system is based on the focus and scanning of low energy, hard x-rays such as those emanating from table top copper or molybdenum sources. The x-rays are focused into a narrow and intense line image which can be swept onto targets that fluoresce secondary x-ray radiation. By monitoring the secondary radiation intensity and comparing it with the focused x-ray image's position as it is swept over the target edge, the position of the target edge relative to the focused image can be determined. The present system has a resolution of 0.5 micron, which has been shown to be limited by bearing backlash (or 'yaw' error) in the linear translation table. Its use has been demonstrated in the presence of an open flame with a resultant target temperature in excess of 2000 degrees Fahrenheit (1000 degrees Celsius). Strain measurements have been conducted in a laboratory environment at both room temperature and at a specimen temperature of 1300 degrees Fahrenheit, with an accuracy of within 20 microstrain (primarily a function of the 0.5 micron resolution limit). The main advantage of the technique lies in the penetrating, non-refractive nature of x-rays, which are virtually immune to the presence of refracting gas layers, smoke, flame or intense thermal radiation.

Luminescence and Scintillation Properties of Czochralski Grown LYGBO Crystals

NASA Astrophysics Data System (ADS)

Fawad, U.; Kim, Hong Joo; Park, H.; Kim, Sunghwan; Khan, Sajid

2016-06-01

Mixed crystals Li6YxGd1-x(BO3)3:Ce3+ (LYGBO) (where, x = 0.0, 0.2, 0.5, 0.8, 1.0) are grown by using Czochralski method with different proportions of Li6Y(BO3)3 and Li6Gd(BO3)3. All crystals are doped with 3 mole% optimized concentrations of Ce3+ ions. The grown crystals are 20-70 mm in length and 5-10 mm in diameter. Detailed sintering and crystal growth procedure is presented in this study. The required phase of the grown crystals is confirmed by powder X-ray diffraction (XRD) analysis. Ultraviolet (UV) photoluminescence and X-ray induced luminescence of the grown crystals at room temperature are measured. Various scintillation properties such as energy resolution, light yield, α/β ratio and fluorescence decay time under the excitation by 137Cs γ-ray and 241Am particles are also presented.

High Pressure X-Ray Crystallography With the Diamond Cell at NIST/NBS

PubMed Central

Piermarini, Gasper J.

2001-01-01

Scientists in the Crystallography Section at NIST/NBS made several outstanding contributions which greatly promoted the development and advancement of high pressure x-ray crystallography during the second-half of the 20th century. These milestone achievements or “firsts” included: (1) the invention of the lever-arm type diamond anvil cell (DAC) in 1958; (2) the development of DAC technology for powder x-ray diffraction at high pressure in 1960; (3) the introduction of DAC methodology for single crystal x-ray diffraction at high pressure in 1964; (4) the invention of the optical fluorescence ruby method of pressure measurement in 1971; and (5) the discovery of hydrostatic pressure-transmitting media useful to unprecedented pressures for that time. These achievements provided the spark that ignited the explosion of activity in high pressure research that occurred in laboratories throughout the world during the latter part of the 20th century. It is still going on, unabated, today. An estimated 5000 DACs were built during the last 40 years. PMID:27500054

Valence electronic structure of Ni in Ni Si alloys from relative K X-ray intensity studies

NASA Astrophysics Data System (ADS)

Kalayci, Y.; Aydinuraz, A.; Tugluoglu, B.; Mutlu, R. H.

2007-02-01

The Kβ-to-Kα X-ray intensity ratio of Ni in Ni 3Si, Ni 2Si and NiSi has been determined by energy dispersive X-ray fluorescence technique. It is found that the intensity ratio of Ni decreases from pure Ni to Ni 2Si and then increases from Ni 2Si to NiSi, in good agreement with the electronic structure calculations cited in the literature. We have also performed band structure calculations for pure Ni in various atomic configurations by means of linear muffin-tin orbital method and used this data with the normalized theoretical intensity ratios cited in the literature to estimate the 3d-occupation numbers of Ni in Ni-Si alloys. It is emphasized that investigation of alloying effect in terms of X-ray intensity ratios should be carried out for the stoichiometric alloys in order to make reliable and quantitative comparisons between theory and experiment in transition metal alloys.

Separation of detector non-linearity issues and multiple ionization satellites in alpha-particle PIXE

NASA Astrophysics Data System (ADS)

Campbell, John L.; Ganly, Brianna; Heirwegh, Christopher M.; Maxwell, John A.

2018-01-01

Multiple ionization satellites are prominent features in X-ray spectra induced by MeV energy alpha particles. It follows that the accuracy of PIXE analysis using alpha particles can be improved if these features are explicitly incorporated in the peak model description when fitting the spectra with GUPIX or other codes for least-squares fitting PIXE spectra and extracting element concentrations. A method for this incorporation is described and is tested using spectra recorded on Mars by the Curiosity rover's alpha particle X-ray spectrometer. These spectra are induced by both PIXE and X-ray fluorescence, resulting in a spectral energy range from ∼1 to ∼25 keV. This range is valuable in determining the energy-channel calibration, which departs from linearity at low X-ray energies. It makes it possible to separate the effects of the satellites from an instrumental non-linearity component. The quality of least-squares spectrum fits is significantly improved, raising the level of confidence in analytical results from alpha-induced PIXE.

A top-down method to fabricate SrAl2O4:Eu2+,Dy3+ nanosheets from commercial blocky phosphors

NASA Astrophysics Data System (ADS)

Zhang, Haoran; Xue, Zhiping; Lei, Bingfu; Dong, Hanwu; Zhang, Haiming; Deng, Suqing; Zheng, Mingtao; Liu, Yingliang; Xiao, Yong

2014-09-01

By using commercial SrAl2O4:Eu2+,Dy3+ phosphor as raw material, we have developed a novel and simple top-down method to fabricate SrAl2O4:Eu2+,Dy3+ nanosheets that are useful for potential practical applications, especially as fluorescent labels for biomolecules and mechano-optical nano-devices. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDX) results demonstrate that the treated samples are still pure-phase of SrAl2O4:Eu2+,Dy3+. The field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) results indicate that the treated SrAl2O4:Eu2+,Dy3+ phosphors are built up by nanosheets bundles. Excitation and emission spectra, afterglow emission spectra and decay curves are used to analyze the luminescence properties of SrAl2O4:Eu2+,Dy3+ nanosheets, and the results show that, compared with commercial samples, the treated samples show similar spectra characteristic including the spectra shapes and the band position. Furthermore, the fluorescence and afterglow intensity of SrAl2O4:Eu2+,Dy3+ nanosheets can be tuned linearly by changing the circumstance temperatures, which further indicates its potential applications in fiber-optical thermometer materials.

Localization and distribution of Zn and Fe in grains of biofortified bread wheat lines through micro- and triaxial-X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Cardoso, P.; Mateus, T. C.; Velu, G.; Singh, R. P.; Santos, J. P.; Carvalho, M. L.; Lourenço, V. M.; Lidon, F.; Reboredo, F.; Guerra, M.

2018-03-01

X-ray fluorescence analysis has been performed in wheat grains from a field trial where some biofortified and non-biofortified wheat varieties were subjected to Zn biofortification through soil fertilizer application. A set of ten biofortified and non-biofortified wheat varieties developed at the International Maize and Wheat Improvement Center, Mexico, were used for this study. Two analytical methods were employed to investigate the contents and localization of the trace metals Zn and Fe within the grains, one with polarized monochromatic X-rays for lower limits of detection, and another featuring polycapillary lenses for micrometric beam size (μ-EDXRF). Elemental maps were obtained with μ-EDXRF allowing for the study of Zn and Fe localization in plants grown in normal and Zn-enriched soil. It is acknowledged that the biofortification procedures result in around 30% average increase in overall Zn concentration when compared to other high Zn genotypes grown in normal soil. A genotypic ranking was performed taking into account the influence of the measurement methods and field conditions and the obtained results show that two of the top three varieties regarding zinc contents also rank among the top three in terms of Fe concentration. Elemental mapping analysis seems to favor the use of integral flour for the manufacture of bread and pasta products, as the bran retains most of the minerals.

Suzaku Observation of Strong Fluorescent Iron Line Emission from the Young Stellar Object V1647 Ori during Its New X-ray Outburst

NASA Technical Reports Server (NTRS)

Hamaguchi, Kenji; Grosso, Nicolas; Kastner, Joel H.; Weintraub, David A.; Richmond, Michael

2009-01-01

The Suzaku X-ray satellite observed the young stellar object V1647 Ori on 2008 October 8 during the new mass accretion outburst reported in August 2008. During the 87 ksec observation with a net exposure of 40 ks, V1647 Ori showed a. high level of X-ray emission with a gradual decrease in flux by a factor of 5 and then displayed an abrupt flux increase by an order of magnitude. Such enhanced X-ray variability was also seen in XMM-Newton observations in 2004 and 2005 during the 2003-2005 outburst, but has rarely been observed for other young stellar objects. The spectrum clearly displays emission from Helium-like iron, which is a signature of hot plasma (kT approx.5 keV). It also shows a fluorescent iron Ka line with a remarkably large equivalent width of approx. 600 eV. Such a, large equivalent width indicates that a part of the incident X-ray emission that irradiates the circumstellar material and/or the stellar surface is hidden from our line of sight. XMM-Newton spectra during the 2003-2005 outburst did not show a strong fluorescent iron Ka line ; so that the structure of the circumstellar gas very close to the stellar core that absorbs and re-emits X-ray emission from the central object may have changed in between 2005 and 2008. This phenomenon may be related to changes in the infrared morphology of McNeil's nebula between 2004 and 2008.

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

PubMed

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

2017-08-01

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

Combined SRCT & FXCT - The next steps

NASA Astrophysics Data System (ADS)

Hall, C.; Acres, R. G.; Winnett, A.; Wang, F.

2016-03-01

One of the goals in developing synchrotron radiation x-ray computed tomography (SRCT) for biomedical specimens, is allowing particular tissues and cell types to be marked in the images. This is equivalent to the staining in histology, which enables researchers to visualise and measure tissue structure and biochemical processes within the specimen. Some progress in this direction for SRCT is being made, using a variety of contrast agents that alter the natural x-ray attenuation of the marked tissue [1]. However there are limits to the usefulness of these attenuation altering techniques. Often high concentrations of potentially disruptive chemicals are required with reduced compatibility for in-vivo studies. Another image highlighting technique which might prove more sensitive is x-ray fluorescence imaging. In this case usually endogenous elemental markers are visualised. We would like to develop a lower resolution, but wider field of view means of three-dimensional (3-D) fluorescence imaging compatible with SRCT. We have previously proposed a technique in which x-ray fluorescence CT (FXCT) and SRCT data can be collected simultaneously [2]. This work resulted in proof of concept modelling, and a simple experiment test system. We show data here which demonstrate a two-dimensional (2-D) reconstruction of an iodine fluorescence map from a phantom. Measurements were performed with a fixed beam modulating mask using the Imaging and Medical beam line (IMBL) at the Australian Synchrotron. Fluorescence data was obtained during a CT scan using a single point detector, while transmission data was simultaneously collected using an area detector. A maximum likelihood expectation maximisation (MLEM) iterative algorithm was used to reconstruct the fluorescence map. We report on technique development and now believe compressive sensing (CS) imaging techniques suit SRCT and may overcome the issues encountered so far in combining SRCT and FXCT.

Kα resonance fluorescence in Al, Ti, Cu and potential applications for X-ray sources

NASA Astrophysics Data System (ADS)

Nahar, Sultana N.; Pradhan, Anil K.

2015-04-01

The Kα resonance fluorescence (RFL) effect via photoabsorptions of inner shell electrons as the element goes through multiple ionization states is studied. We demonstrate that the resonances observed recently in Kα (1s-2p) fluorescence in aluminum plasmas by using a high-intensity X-ray free-electron laser [1] are basically K-shell resonances in hollow atoms going through multiple ionization states at resonant energies as predicted earlier for gold and iron ions [2]. These resonances are formed below the K-shell ionization edge and shift toward higher energies with ionization states, as observed. Fluorescence emission intensities depend on transition probabilities for each ionization stage of the given element for all possible Kα (1 s → 2 p) transition arrays. The present calculations for resonant photoabsorptions of Kα photons in Al have reproduced experimentally observed features. Resonant cross sections and absorption coefficients are presented for possible observation of Kα RFL in the resonant energy ranges of 4.5-5.0 keV for Ti ions and 8.0-8.7 keV for Cu ions respectively. We suggest that theoretically the Kα RFL process may be driven to enhance the Auger cycle by a twin-beam monochromatic X-ray source, tuned to the K-edge and Kα energies, with potential applications such as the development of narrow-band biomedical X-ray devices.

Improving the Raster Scanning Methods used with X-ray Fluorescence to See the Ancient Greek Text of Archimedes (SULI Paper)

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

Griffin, Isabella B.; /Norfolk State U. /SLAC, SSRL

2006-01-04

X-ray fluorescence is being used to detect the ancient Greek copy of Archimedes work. The copy of Archimedes text was erased with a weak acid and written over to make a prayer book in the Middle Ages. The ancient parchment, made of goat skin, has on it some of Archimedes most valuable writings. The ink in the text contains iron which will fluoresce under x-ray radiation. My research project deals with the scanning and imaging process. The palimpsest is put in a stage that moves in a raster format. As the beam hits the parchment, a germanium detector detects themore » iron atoms and discriminates against other elements. Since the computer scans in both forwards and backwards directions, it is imperative that each row of data lines up exactly on top of the next row. There are several parameters to consider when scanning the parchment. These parameters include: speed, count time, shutter time, x-number of points, and acceleration. Formulas were made to relate these parameters together. During the actual beam time of this project, the scanning was very slow going; it took 30 hours to scan 1/2 of a page. Using the formulas, the scientists doubled distance and speed to scan the parchment faster; however, the grey scaled data was not lined up properly causing the images to look blurred. My project was is to find out why doubling the parameters caused blurred images, and to fix the problem if it is fixable.« less

Microporous Cd(II) metal-organic framework as fluorescent sensor for nitroaromatic explosives at the sub-ppm level

NASA Astrophysics Data System (ADS)

Wang, Xing-Po; Han, Lu-Lu; Wang, Zhi; Guo, Ling-Yu; Sun, Di

2016-03-01

A novel Cd(II) metal-organic framework (MOF) based on a rigid biphenyltetracarboxylic acid, [Cd4(bptc)2(DMA)4(H2O)2·4DMA] (1) was successfully synthesized under the solvothermal condition and characterized by single-crystal X-ray diffraction and further consolidated by elemental analyses, powder X-ray diffraction (PXRD), infrared spectra (IR) and luminescent measurements. Single crystal X-ray diffraction analysis reveals that compound 1 is 4-connected PtS (Point symbol: {42·84}) network based on [Cd2(COO)4] secondary building units (SBUs). Its inherent porous and emissive characteristics make them to be a suitable fluorescent probe to sense small solvents and nitroaromatic explosives. Compound 1 shows obviously solvent-dependent emissive behaviors, especially for acetone with very high fluorescence quenching effect. Moreover, compound 1 displays excellent sensing of nitroaromatic explosives at sub-ppm level, giving a detection limit of 0.43 ppm and 0.37 ppm for nitrobenzene (NB) and p-nitrotoluene (PNT), respectively. This shows this Cd(II) MOF can be used as fluorescence probe for the detection of nitroaromatic explosives.

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

Wilson, Matthew D., E-mail: Matt.Wilson@stfc.ac.uk; Seller, Paul; Veale, Matthew C.

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

[Method of fused sample preparation after nitrify-determination of primary and minor elements in manganese ore by X-ray fluorescence spectrometry].

PubMed

Song, Yi; Guo, Fen; Gu, Song-hai

2007-02-01

Eight components, i. e. Mn, SiO2, Fe, P, Al2O3, CaO, MgO and S, in manganese ore were determined by X-ray fluorescence spectrometer. Because manganese ore sample releases a lot of air bubbles during fusion which effect accuracy and reproducibility of determination, nitric acid was added to the sample to destroy organic matter before fusion by the mixture flux at 1000 degrees C. This method solved the problem that the flux splashed during fusion because organic matter volatilized brought out a lot of air bubbles, eliminated particle size effects and mineral effect, while solved the problem of volatilization of sulfur during fusion. The experiments for the selection of the sample preparation conditions, i. e. fusion flux, fusion time and volume of HNO3, were carried out. The matrix effects on absorption and enhancement were corrected by variable theoretical alpha coefficient to expand the range of determination. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

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

NASA Technical Reports Server (NTRS)

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

1977-01-01

The X-ray spectrum of Hercules X-1 was observed in the energy range 2-24 keV from August 29 to September 3, 1975. A broad iron line feature is observed in the normal high state spectrum. The line equivalent width is given along with its full-width-half-maximum energy. Iron line fluorescence from an opaque, cool shell of material at the Alfven surface provides the necessary luminosity in this feature. The line energy width can be due to Doppler broadening if the shell is forced to corotate with the pulsar at a radius 800 million cm. Implications of this model regarding physical conditions near Her X-1 are discussed.

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

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

Chandra Captures Venus In A Whole New Light

NASA Astrophysics Data System (ADS)

2001-11-01

Scientists have captured the first X-ray view of Venus using NASA's Chandra X-ray Observatory. The observations provide new information about the atmosphere of Venus and open a new window for examining Earth's sister planet. Venus in X-rays looks similar to Venus in visible light, but there are important differences. The optically visible Venus is due to the reflection of sunlight and, for the relative positions of Venus, Earth and Sun during these observations, shows a uniform half-crescent that is brightest toward the middle. The X-ray Venus is slightly less than a half-crescent and brighter on the limbs. The differences are due to the processes by which Venus shines in visible and X-ray light. The X-rays from Venus are produced by fluorescence, rather than reflection. Solar X-rays bombard the atmosphere of Venus, knock electrons out of the inner parts of the atoms, and excite the atoms to a higher energy level. The atoms almost immediately return to their lower energy state with the emission of a fluorescent X-ray. A similar process involving ultraviolet light produces the visible light from fluorescent lamps. For Venus, most of the fluorescent X-rays come from oxygen and carbon atoms between 120 and 140 kilometers (74 to 87 miles) above the planet's surface. In contrast, the optical light is reflected from clouds at a height of 50 to 70 kilometers (31 to 43 miles). As a result, Venus' Sun-lit hemisphere appears surrounded by an almost-transparent luminous shell in X-rays. Venus looks brightest at the limb since more luminous material is there. Venus X-ray/Optical Composite of Venus Credit: Xray: NASA/CXC/MPE/K.Dennerl et al., Optical: Konrad Dennerl "This opens up the exciting possibility of using X-ray observations to study regions of the atmosphere of Venus that are difficult to investigate by other means," said Konrad Dennerl of the Max Planck Institute for Extraterrestrial Physics in Garching, Germany, leader of an international team of scientists that conducted the research. The Chandra observation of Venus was also a technological tour de force. The angular separation of Venus from the Sun, as seen from Earth, never exceeds 48 degrees. This relative proximity has prevented star trackers and cameras on other X-ray astronomy satellites from locking onto guide stars and pointing steadily in the direction of Venus to perform such an observation. Venus was observed on Jan. 10, 2001, with the Advanced CCD Imaging Spectrometer (ACIS) detector plus the Low Energy Transmission Grating and on Jan. 13, 2001, with the ACIS alone. Other members of the team were Vadim Burwitz and Jakob Engelhauser, Max Planck Institute; Carey Lisse, University of Maryland, College Park; and Scott Wolk, Harvard-Smithsonian Center for Astrophysics, Cambridge, Mass. These results were presented at this week's "New Visions of X-ray universe in the XMM-Newton and Chandra Era" symposium in Noordwijk, Netherlands. The Low Energy Transmission Grating was built by the Space Research Organization of the Netherlands and the Max Planck Institute, and the ACIS instrument was developed for NASA by The Pennsylvania State University, University Park, and the Massachusetts Institute of Technology (MIT), Cambridge. NASA's Marshall Space Flight Center in Huntsville, Ala., manages the Chandra program. The Smithsonian's Chandra X-ray Center controls science and flight operations from Cambridge, Mass.

CheMin Instrument Performance and Calibration on Mars

NASA Technical Reports Server (NTRS)

Vaniman, D. T.; Blake, D. F.; Morookian, J. M.; Yen, A. S.; Ming, D. W.; Morris, R. V.; Achilles, C. N.; Bish, D. L.; Chipera, S. J.; Morrison, S. M.;

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

PubMed

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

2012-05-15

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

Depth profiling of marker layers using x-ray waveguide structures

NASA Astrophysics Data System (ADS)

Gupta, Ajay; Rajput, Parasmani; Saraiya, Amit; Reddy, V. R.; Gupta, Mukul; Bernstorff, Sigrid; Amenitsch, H.

2005-08-01

It is demonstrated that x-ray waveguide structures can be used for depth profiling of a marker layer inside the guiding layer with an accuracy of better than 0.2 nm. A combination of x-ray fluorescence and x-ray reflectivity measurements can provide detailed information about the structure of the guiding layer. The position and thickness of the marker layer affect different aspects of the angle-dependent x-ray fluorescence pattern, thus making it possible to determine the structure of the marker layer in an unambiguous manner. As an example, effects of swift heavy ion irradiation on a Si/M/Si trilayer ( M=Fe , W), forming the cavity of the waveguide structure, have been studied. It is found that in accordance with the prediction of thermal spike model, Fe is much more sensitive to swift heavy ion induced modifications as compared to W, even in thin film form. However, a clear evidence of movement of the Fe marker layer towards the surface is observed after irradiation, which cannot be understood in terms of the thermal spike model alone.

Quantitative evaluation of the pulmonary microdistribution of TiO2 nanoparticles using X-ray fluorescence microscopy after intratracheal administration with a microsprayer in rats.

PubMed

Zhang, Guihua; Shinohara, Naohide; Kano, Hirokazu; Senoh, Hideki; Suzuki, Masaaki; Sasaki, Takeshi; Fukushima, Shoji; Gamo, Masashi

2015-06-01

The unevenness of pulmonary nanoparticle (NP) distribution, which hinders the establishment of an absolute dose-response relationship, has been described as one of the limitations of intratracheal administration techniques for toxicological assessment of inhaled NPs. Quantification of the NP microdistribution would facilitate the establishment of a concentration-response relationship in localized regions of the lung; however, such quantitative methods have not been reported. Here, we established a quantitative method for evaluating pulmonary TiO2 NP microdistribution in rats using X-ray fluorescence microscopy. Ti intensity in lung sections from rats intratracheally administered 10 mg kg(-1) TiO2 NPs with a microsprayer was measured using X-ray fluorescence with a 100 µm beam size. Ti reference samples were prepared by dropping different concentrations of Ti solutions on glass slide or lung sections of untreated rat. Ti intensity increased linearly with Ti content in the reference samples on both substrates. The detection limit of TiO2 was estimated to be 6.3 ng mm(-2) . The reproducibility was confirmed for measurements done in the short- (2 weeks) and long-term (6 months). The quantitative results of TiO2 NP microdistribution suggested that more TiO2 NPs were distributed in the right caudal and accessory lobes, which are located downstream of the administration direction of the NP suspension, and the lower portion of each lobe. The detection rates of TiO2 NPs were 16.6-25.0%, 5.19-15.6%, 28.6-39.2%, 21.4-38.7% and 10.6-23.2% for lung sections from the right cranial, middle, caudal, accessory and left lobes, respectively. Copyright © 2015 John Wiley & Sons, Ltd.

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 excited with 109Cd. 55Fe will be primarily dedicated to XRD measurements, as it has been already tested for the MARS-XRD development. 109Cd will be used to reinforce the efficiency of 55Fe source in the production of fluorescent X-rays generated in the sample as a consequence of irradiation and to extend the analytical range of elements. Two different detectors will be used in order to increase the total amount of events collected and allow the spatial distribution of events to be recorded as well. The detectors we plan to use are SDD (Silicon Drift Detector) and stand-alone CCD (Coupled Charge Detector). SDD has higher count rate and stability and has been successfully used for XRF applications. CCD is able to record the spatial position of each event of X-ray emission, together with its energy. Therefore, we plan to dedicate this detector to XRD measurements, where the spatial position of the event is directly correlated to the type of crystal through the Bragg's law. A prototype of the instrument will be likely completed by the end of this year.

Micro-X-Ray Fluorescence, Micro-X-Ray Absorption Spectroscopy, and Micro-X-Ray Diffraction Investigation of Lead Speciation after the Addition of Different Phosphorus Amendments to a Smelter-Contaminated Soil

EPA Science Inventory

The stabilization of Pb on additions of P to contaminated soils and mine spoil materials has been well documented. It is clear from the literature that different P sources result in different efficacies of Pb stabilization in the same contaminated material. We hypothesized that...

Symposium LL: Nanowires--Synthesis Properties Assembly and Application

DTIC Science & Technology

2010-09-10

dedicated hard x - ray microscopy beamline is operated in partnership with the Advanced Photon Source to provide fluorescence, diffraction, and...characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X - ray diffraction (XRD) measurements, proving it to be...Investigation of Preferred Growth Direction of GaN Nanorods by Synchrotron X - ray Reciprocal Space Mapping. Yuri Sohn1, Sanghwa Lee1, Chinkyo Kim1 and Dong

Determination of stoichiometry and concentration of trace elements in thin BaxSr1-xTiO3 perovskite layers.

PubMed

Becker, J S; Boulyga, S F

2001-07-01

This paper describes an analytical procedure for determining the stoichiometry of BaxSr1-xTiO3 perovskite layers using inductively coupled plasma mass spectrometry (ICP-MS). The analytical results of mass spectrometry measurements are compared to those of X-ray fluorescence analysis (XRF). The performance and the limits of solid-state mass spectrometry analytical methods for the surface analysis of thin BaxSr1-xTiO3 perovskite layers sputtered neutral mass spectrometry (SNMS)--are investigated and discussed.

Application toward Confocal Full-Field Microscopic X-ray Absorption Near Edge Structure Spectroscopy.

PubMed

Tack, Pieter; Vekemans, Bart; Laforce, Brecht; Rudloff-Grund, Jennifer; Hernández, Willinton Y; Garrevoet, Jan; Falkenberg, Gerald; Brenker, Frank; Van Der Voort, Pascal; Vincze, Laszlo

2017-02-07

Using X-ray absorption near edge structure (XANES) spectroscopy, information on the local chemical structure and oxidation state of an element of interest can be acquired. Conventionally, this information can be obtained in a spatially resolved manner by scanning a sample through a focused X-ray beam. Recently, full-field methods have been developed to obtain direct 2D chemical state information by imaging a large sample area. These methods are usually in transmission mode, thus restricting the use to thin and transmitting samples. Here, a fluorescence method is displayed using an energy-dispersive pnCCD detector, the SLcam, characterized by measurement times far superior to what is generally applicable. Additionally, this method operates in confocal mode, thus providing direct 3D spatially resolved chemical state information from a selected subvolume of a sample, without the need of rotating a sample. The method is applied to two samples: a gold-supported magnesia catalyst (Au/MgO) and a natural diamond containing Fe-rich inclusions. Both samples provide XANES spectra that can be overlapped with reference XANES spectra, allowing this method to be used for fingerprinting and linear combination analysis of known XANES reference compounds.

Lifetime-vibrational interference effects in resonantly excited x-ray emission spectra of CO

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

Skytt, P.; Glans, P.; Gunnelin, K.

1997-04-01

The parity selection rule for resonant X-ray emission as demonstrated for O{sub 2} and N{sub 2} can be seen as an effect of interference between coherently excited degenerate localized core states. One system where the core state degeneracy is not exact but somewhat lifted was previously studied at ALS, namely the resonant X-ray emission of amino-substituted benzene (aniline). It was shown that the X-ray fluorescence spectrum resulting from excitation of the C1s at the site of the {open_quotes}aminocarbon{close_quotes} could be described in a picture separating the excitation and the emission processes, whereas the spectrum corresponding to the quasi-degenerate carbons couldmore » not. Thus, in this case it was necessary to take interference effects between the quasi-degenerate intermediate core excited states into account in order to obtain agreement between calculations and experiment. The different vibrational levels of core excited states in molecules have energy splittings which are of the same order of magnitude as the natural lifetime broadening of core excitations in the soft X-ray range. Therefore, lifetime-vibrational interference effects are likely to appear and influence the band shapes in resonant X-ray emission spectra. Lifetime-vibrational interference has been studied in non-resonant X-ray emission, and in Auger spectra. In this report the authors discuss results of selectively excited soft X-ray fluorescence spectra of molecules, where they focus on lifetime-interference effects appearing in the band shapes.« less

Novel heterocyclic thiosemicarbazones derivatives as colorimetric and "turn on" fluorescent sensors for fluoride anion sensing employing hydrogen bonding.

PubMed

Ashok Kumar, S L; Saravana Kumar, M; Sreeja, P B; Sreekanth, A

2013-09-01

Two novel heterocyclic thiosemicarbazone derivatives have been synthesized, and characterized, by means of spectroscopic and single crystal X-ray diffraction methods. Their chromophoric-fluorogenic response towards anions in competing solvent dimethyl sulfoxide (DMSO) was studied. The receptor shows selective recognition towards fluoride anion. The binding affinity of the receptors with fluoride anion was calculated using UV-visible and fluorescence spectroscopic techniques. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis and characterization of graphene quantum dots/cobalt ferrite nanocomposite

NASA Astrophysics Data System (ADS)

Ramachandran, Shilpa; Sathishkumar, M.; Kothurkar, Nikhil K.; Senthilkumar, R.

2018-02-01

A facile method has been developed for the synthesis of a graphene quantum dots/cobalt ferrite nanocomposite. Graphene quantum dots (GQDs) were synthesized by a simple bottom-up method using citric acid, followed by the co-precipitation of cobalt ferrite nanoparticles on the graphene quantum dots. The morphology, structural analysis, optical properties, magnetic properties were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis absorption spectroscopy, fluorescence spectroscopy, vibrating sample magnetometry (VSM) measurements. The synthesized nanocomposite showed good fluorescence and superparamagnetic properties, which are important for biomedical applications.

Efficiency of cytogenetic methods in detecting a chromosome rearrangement induced by ionizing radiation in a cultivated chili pepper line (Capsicum baccatum var. pendulum--Solanaceae).

PubMed

Scaldaferro, Marisel A; Grabiele, Mauro; Seijo, J Guillermo; Debat, Humberto; Romero, M Victoria; Ducasse, Daniel A; Prina, Alberto R; Moscone, Eduardo A

2014-01-01

To locate transient chromosome aberrations on a selected pepper cultivar and determine the tracing efficiency of different cytogenetic methods. Seeds from Capsicum baccatum var. pendulum cultivar 'Cayenne' were treated with an acute dose of X-rays (300 Gy) and chromosome aberrations were analysed by different cytogenetic methods [Feulgen, silver staining for nucleolus organizer regions (silver positive nucleolus organizing regions or AgNOR), fluorescent banding, fluorescence in situ hybridization (FISH) and meiotic analysis]. A rearranged chromosome carrying two nucleolus organizing regions (NOR) induced by ionizing radiation was detected in the cultivar, with the occurrence of a small reciprocal exchange between a chromosome of pair no. 1 and another chromosome of pair no. 3, both carrying active NOR in short arms and associated chromomycin A positive/diamidino-phenylindole negative (CMA+/DAPI-) heterochromatin. Meiotic analysis showed a quadrivalent configuration, confirming a reciprocal translocation between two chromosomes. The use of X-rays in Capsicum allowed us to develop and identify a pepper line with structural rearrangements between two NOR-carrying chromosomes. We postulate that all the cytological techniques employed in this research were efficient in the search for chromosome aberrations. Particularly, Feulgen and AgNOR were the most suitable in those cases of transient rearrangements, whereas fluorescent banding and FISH were appropriate for intransitive ones.

IDENTIFICATION OF IRON PHASES IN BIOSOLIDS VIA MOSSBAUER SPECTROSCOPY

EPA Science Inventory

Continuous debate regarding inorganic and organic phases in biosolids as prominent sorbents of metals has yielded limited definitive data. We have demonstrated with X-ray absorption and X-ray fluorescence spectroscopies that metals in biosolids have a significant association with...

Publications - GMC 420 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 420 Publication Details Title: X-Ray fluorescence spectroscopy and 40Ar/39Ar analyses of core more information. Quadrangle(s): Ikpikpuk River; Umiat Bibliographic Reference Shimer, G., 2013, X-Ray

Synchrotron x-ray spectroscopy of EuHN O3 aqueous solutions at high temperatures and pressures and Nb-bearing silicate melt phases coexisting with hydrothermal fluids using a modified hydrothermal diamond anvil cell and rail assembly

USGS Publications Warehouse

Mayanovic, Robert A.; Anderson, Alan J.; Bassett, William A.; Chou, I.-Ming

2007-01-01

A modified hydrothermal diamond anvil cell (HDAC) rail assembly has been constructed for making synchrotron x-ray absorption spectroscopy, x-ray fluorescence, and x-ray mapping measurements on fluids or solid phases in contact with hydrothermal fluids up to ???900??C and 700 MPa. The diamond anvils of the HDAC are modified by laser milling grooves or holes, for the reduction of attenuation of incident and fluorescent x rays and sample cavities. The modified HDAC rail assembly has flexibility in design for measurement of light elements at low concentrations or heavy elements at trace levels in the sample and the capability to probe minute individual phases of a multiphase fluid-based system using focused x-ray microbeam. The supporting rail allows for uniform translation of the HDAC, rotation and tilt stages, and a focusing mirror, which is used to illuminate the sample for visual observation using a microscope, relative to the direction of the incident x-ray beam. A structure study of Eu(III) aqua ion behavior in high-temperature aqueous solutions and a study of Nb partitioning and coordination in a silicate melt in contact with a hydrothermal fluid are described as applications utilizing the modified HDAC rail assembly. ?? 2007 American Institute of Physics.

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.

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

NASA Astrophysics Data System (ADS)

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

2015-08-01

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

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.

Fluorescent Approaches to High Throughput Crystallography

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Forsythe, Elizabeth; Achari, Amiruddha

2005-01-01

X-ray crystallography remains the primary method for determining the structure of macromolecules. The first requirement is to have crystals, and obtaining them is often the rate-limiting step. The numbers of crystallization trials that are set up for any one protein for structural genomics, and the rate at which they are being set up, now overwhelm the ability for strictly human analysis of the results. Automated analysis methods are now being implemented with varying degrees of success, but these typically cannot reliably extract intermediate results. By covalently modifying a subpopulation, less than or = 1 %, of a macromolecule solution with a fluorescent probe, the labeled material will add to a growing crystal as a microheterogeneous growth unit. Labeling procedures can be readily incorporated into the final stages of purification. The covalently attached probe will concentrate in the crystal relative to the solution, and under fluorescent illumination the crystals show up as bright objects against a dark background. As crystalline packing is more dense than amorphous precipitate, the fluorescence intensity can be used as a guide in distinguishing different types of precipitated phases, even in the absence of obvious crystalline features, widening the available potential lead conditions in the absence of clear "hits." Non-protein structures, such as salt crystals, will not incorporate the probe and will not show up under fluorescent illumination. Also, brightly fluorescent crystals are readily found against less fluorescent precipitated phases, which under white light illumination may serve to obscure the crystals. Automated image analysis to find crystals should be greatly facilitated, without having to first define crystallization drop boundaries and by having the protein or protein structures all that show up. The trace fluorescently labeled crystals will also emit with sufficient intensity to aid in the automation of crystal alignment using relatively low cost optics, further increasing throughput at synchrotrons. Preliminary experiments show that the presence of the fluorescent probe does not affect the nucleation process or the quality of the X-ray data obtained.

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.

Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

PubMed Central

Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

2016-01-01

For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

New contrasts for x-ray imaging and synergy with optical imaging

NASA Astrophysics Data System (ADS)

Wang, Ge

2017-02-01

Due to its penetrating power, fine resolution, unique contrast, high-speed, and cost-effectiveness, x-ray imaging is one of the earliest and most popular imaging modalities in biomedical applications. Current x-ray radiographs and CT images are mostly on gray-scale, since they reflect overall energy attenuation. Recent advances in x-ray detection, contrast agent, and image reconstruction technologies have changed our perception and expectation of x-ray imaging capabilities, and generated an increasing interest in imaging biological soft tissues in terms of energy-sensitive material decomposition, phase-contrast, small angle scattering (also referred to as dark-field), x-ray fluorescence and luminescence properties. These are especially relevant to preclinical and mesoscopic studies, and potentially mendable for hybridization with optical molecular tomography. In this article, we review new x-ray imaging techniques as related to optical imaging, suggest some combined x-ray and optical imaging schemes, and discuss our ideas on micro-modulated x-ray luminescence tomography (MXLT) and x-ray modulated opto-genetics (X-Optogenetics).

M shell X-ray production cross sections and fluorescence yields for the elements with 71 <= Z <= 92 using 5.96 keV photons

NASA Astrophysics Data System (ADS)

Puri, S.; Mehta, D.; Chand, B.; Singh, Nirmal; Mangal, P. C.; Trehan, P. N.

1993-03-01

Total M X-ray production (XRP) cross sections for ten elements in the atomic number region 71 ≤ Z ≤ 92 were measured at 5.96 keV incident photon energy. The average M shell fluorescence yields < overlineωM> have also been computed using the present measured cross section values and the theoretical M shell photoionisation cross sections. The results are compared with theoretical values.

Controlling Corrosion in Defence Equipment - Technical Meeting,

DTIC Science & Technology

1985-10-01

methods identify elements. (c) IR absorption spectroscopy. % e The identifies radicals, sometimes compounds. X-ray fluorescence and atomic absorption ...components from this radio. There were 100 sets all with defective - silver plating, with a total value of $5 million. A method of refurbishment was...Assemblies from the FiiC Aircraft Slides of a corroded heat exchanger assembly were shown. A method of refurbishment was suggested. Estimated saving - $0.5

Intracellular in situ labeling of TiO 2 nanoparticles for fluorescence microscopy detection

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

Brown, Koshonna; Thurn, Ted; Xin, Lun

Titanium dioxide (TiO 2) nanoparticles are produced for many different purposes, including development of therapeutic and diagnostic nanoparticles for cancer detection and treatment, drug delivery, induction of DNA double-strand breaks, and imaging of specific cells and subcellular structures. Currently, the use of optical microscopy, an imaging technique most accessible to biology and medical pathology, to detect TiO 2 nanoparticles in cells and tissues ex vivo is limited with low detection limits, while more sensitive imaging methods (transmission electron microscopy, X-ray fluorescence microscopy, etc.) have low throughput and technical and operational complications. In this paper, we describe two in situ posttreatmentmore » labeling approaches to stain TiO 2 nanoparticles taken up by the cells. The first approach utilizes fluorescent biotin and fluorescent streptavidin to label the nanoparticles before and after cellular uptake; the second approach is based on the copper-catalyzed azide-alkyne cycloaddition, the so-called Click chemistry, for labeling and detection of azide-conjugated TiO 2 nanoparticles with alkyneconjugated fluorescent dyes such as Alexa Fluor 488. To confirm that optical fluorescence signals of these nanoparticles match the distribution of the Ti element, we used synchrotron X-ray fluorescence microscopy (XFM) at the Advanced Photon Source at Argonne National Laboratory. Titanium-specific XFM showed excellent overlap with the location of optical fluorescence detected by confocal microscopy. Finally and therefore, future experiments with TiO 2 nanoparticles may safely rely on confocal microscopy after in situ nanoparticle labeling using approaches described here.« less

Intracellular in situ labeling of TiO 2 nanoparticles for fluorescence microscopy detection

DOE PAGES

Brown, Koshonna; Thurn, Ted; Xin, Lun; ...

2017-07-19

Titanium dioxide (TiO 2) nanoparticles are produced for many different purposes, including development of therapeutic and diagnostic nanoparticles for cancer detection and treatment, drug delivery, induction of DNA double-strand breaks, and imaging of specific cells and subcellular structures. Currently, the use of optical microscopy, an imaging technique most accessible to biology and medical pathology, to detect TiO 2 nanoparticles in cells and tissues ex vivo is limited with low detection limits, while more sensitive imaging methods (transmission electron microscopy, X-ray fluorescence microscopy, etc.) have low throughput and technical and operational complications. In this paper, we describe two in situ posttreatmentmore » labeling approaches to stain TiO 2 nanoparticles taken up by the cells. The first approach utilizes fluorescent biotin and fluorescent streptavidin to label the nanoparticles before and after cellular uptake; the second approach is based on the copper-catalyzed azide-alkyne cycloaddition, the so-called Click chemistry, for labeling and detection of azide-conjugated TiO 2 nanoparticles with alkyneconjugated fluorescent dyes such as Alexa Fluor 488. To confirm that optical fluorescence signals of these nanoparticles match the distribution of the Ti element, we used synchrotron X-ray fluorescence microscopy (XFM) at the Advanced Photon Source at Argonne National Laboratory. Titanium-specific XFM showed excellent overlap with the location of optical fluorescence detected by confocal microscopy. Finally and therefore, future experiments with TiO 2 nanoparticles may safely rely on confocal microscopy after in situ nanoparticle labeling using approaches described here.« less