Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

International Nuclear Information System (INIS)

Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

2013-01-01

A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Ray, N.B.

1977-01-01

The principle, instrument and procedure of X-ray fluorescence spectrometry are described. It is a rapid, simple and sensitive method for the trace analysis of elements from sodium to uranium in powder, liquid or metal samples. (M.G.B.)

X-ray spectrometry with synchrotron radiation; Roentgenspektrometrie mit Synchrotronstrahlung

Energy Technology Data Exchange (ETDEWEB)

Mueller, Matthias [Physikalisch-Technische Bundesanstalt (PTB), Berlin (Germany). Arbeitsgruppe ' Roentgen- und IR-Spektrometrie' ; Gerlach, Martin; Holfelder, Ina; Hoenicke, Philipp; Lubeck, Janin; Nutsch, Andreas; Pollakowski, Beatrix; Streeck, Cornelia; Unterumsberger, Rainer; Weser, Jan; Beckhoff, Burkhard

2014-12-15

The X-ray spectrometry of the PTB at the BESSY II storage ring with radiation in the range from 78 eV to 10.5 keV is described. After a description of the instrumentation development reference-sample free X-ray fluorescence analysis, the determination of fundamental atomic parameters, X-ray fluorescence analysis under glance-angle incidence, highly-resolving absorption spectrometry, and emission spectrometry are considered. Finally liquid cells and in-situ measurement techniques are described. (HSI)

Energy Dispersive Spectrometry and Quantitative Analysis Short Course. Introduction to X-ray Energy Dispersive Spectrometry and Quantitative Analysis

Science.gov (United States)

Carpenter, Paul; Curreri, Peter A. (Technical Monitor)

2002-01-01

This course will cover practical applications of the energy-dispersive spectrometer (EDS) to x-ray microanalysis. Topics covered will include detector technology, advances in pulse processing, resolution and performance monitoring, detector modeling, peak deconvolution and fitting, qualitative and quantitative analysis, compositional mapping, and standards. An emphasis will be placed on use of the EDS for quantitative analysis, with discussion of typical problems encountered in the analysis of a wide range of materials and sample geometries.

Quantitative energy-dispersive electron probe X-ray microanalysis ...

Indian Academy of Sciences (India)

Abstract. An energy-dispersive electron probe X-ray microanalysis (ED-EPMA) technique us- ing an energy-dispersive X-ray detector with an ultra-thin window, designated as low-Z particle. EPMA, has been developed. The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements such ...

The (CuGaSe{sub 2}){sub 1-x}(MgSe){sub x} alloy system (0{<=}x{<=}0.5): X-ray diffraction, energy dispersive spectrometry and differential thermal analysis

Energy Technology Data Exchange (ETDEWEB)

Grima Gallardo, P.; Munoz, M.; Ruiz, J. [Centro de Estudios en Semiconductores (C.E.S.), Dpto. Fisica, Fac. Ciencias, La Hechicera, Merida (Venezuela); Delgado, G.E. [Laboratorio de Cristalografia, Dpto. Quimica, Fac. Ciencias, Universidad de Los Andes, Merida 5101 (Venezuela); Briceno, J.M. [Laboratorio de Analisis Quimico y Estructural (LAQUEM), Dpto. Fisica, Fac. Ciencias, La Hechicera, Merida (Venezuela)

2004-07-01

The (CuGaSe{sub 2}){sub 1-x}(MgSe){sub x} alloy system (0<x{<=}0.5) was investigated using X-ray powder diffraction, energy dispersion spectrometry and differential thermal analysis. The solubility of MgSe in CuGaSe{sub 2} was found to be nearly complete for all the compositions studied, although traces of MgSe appear as a secondary phase at x{>=}0.15. All the alloys showed the chalcopyrite structure and the lattice parameters of the unit cell do not follow a linear behavior but showed a soft local maximum at x {proportional_to} 0.15. In the single-phase field, the increasing behavior of the lattice parameters can be reproduced using an extension for quaternary alloys of Jaffe and Zunger's model for chalcopyrites. (copyright 2004 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Assessment of coal and ash environmental impact with the use of gamma- and X-ray spectrometry

International Nuclear Information System (INIS)

Kierzek, J.; Malozewska-Bucko, B.; Bukowski, P.; Parus, J.L.; Ciurapisnki, A.; Zaras, S.; Kunach, B.; Wiland, K.

1999-01-01

Gamma-ray spectrometry (GS), energy dispersive X-ray fluorescence (EDXRF) analysis methods and wavelength dispersive X-ray fluorescence (WDXRF) were applied for the studies of some coal components, e.g., sulphur, light and heavy metal element concentrations and naturally occurring radioactive isotope contents. Hundred fifty coal samples originating mostly from eight different coal mines from Upper Silesian Coal Basin and 150 samples of ash obtained from these coal samples in laboratory by total combustion at final temperature of 820 deg C, were analyzed. Such comparative analyses can be helpful in selection of most suitable kind of coal for burning in electrical power and heat plants to minimize the environmental pollution. (author)

X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Vries, J.L. de.

1976-01-01

The seventh edition of Philips' Review of Literature on x-ray fluorescence spectrometry starts with a list of conference proceedings on the subject, organised by the Philips organisation at regular intervals in various European countries. It is followed by a list of bulletins. The bibliography is subdivided according to spectra, equipment, applications and absorption analysis

Wavelength Dispersive X-ray Fluorescence Spectrometry for the Analysis of Organic Polymer Film

International Nuclear Information System (INIS)

Choi, Yong Suk; Park, Yong Joon; Kim, Jong Yun

2008-01-01

Recently, many studies have been focused on the thin films because there are numerous industrial processes relevant to thin films such as fuel cells, sensors, lubricants, coatings, and so on. Physical and chemical properties of solid surface have been modified by ultra-thin coatings such as Langmuir-Blodgett (LB) method with a variety of types of organic functional materials for the specific purposes in many applications. In addition, the layer-by-layer technique using polyelectrolyte films are now of interest as biosensors, electrochromic and electroluminescent devices, etc. In general, several methods such as X-ray or neutron reflectivity, and quartz crystal microbalance (QCM) have been utilized for the thin film analysis. These optical techniques can measure the film thicknesses up to hundreds of nanometers while X-ray photoelectron spectroscopy is widely used to study a few nanometers thick films. Other methods such as X-ray Photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atom force microscopy (AFM) have also been used in the film analysis in spite of some disadvantages for each method. X-ray fluorescence (XRF) has long been used as a rapid and simple analytical tool for the analysis of elemental composition of materials. XRF technique is suitable for on-line or in-line real-time monitoring because it is a non-destructive and rapid analysis with good precision and good accuracy at low cost. The aim of this work is to develop a new analytical technique for the quantitative analysis of polymer film on metal substrate. In the present study, Compton peak profile was investigated under different experimental conditions by using wavelength-dispersive XRF (WD-XRF). Compared to energy-dispersive XRF (ED-XRF), WD-XRF is more adequate in an accurate quantitative analysis of thin organic film

Diagnostic X-ray spectrometry using a commercial CdZnTe detector

International Nuclear Information System (INIS)

Becker, P.H.B.

1998-01-01

X ray spectrometry using Ge or Si detectors is an established tool to measure characterization parameters of X-ray beams. This work describes how a commercial CdZnTe was used to perform diagnostic X-ray spectrometry. Spectra were measured for two X-ray machines and compared with similar data found in the literature with an agreement of 2% rms

X-ray spectrometry for preventive conservation of cultural heritage

Indian Academy of Sciences (India)

Analytical chemistry does play a key role in the chemical characterization of the environment and it appears that X-ray spectrometry, in its many forms, is one of the most relevant analytical techniques in preventive conservation, as it is in cultural heritage research in general. X-ray spectrometry has indeed been the method ...

Cu,Cr and As determination in preserved woods (Eucalyptus ssp.) by X-ray fluorescence spectrometries

International Nuclear Information System (INIS)

Pereira Junior, Sergio Matias

2014-01-01

Brazil produces around 2.2 millions of cubic meters of treated wood to meet the annual demand of railway, electric, rural and construction sectors. The most used wood species are eucalyptus (Eucalyptus ssp.) and pine (Pinus ssp.).The treated woods used for poles, sleepers, fence posts and plywoods should be according to Brazilian norms requirements. The most usual wood preservative products used in Brazil are CCA (chromated copper arsenate) and CCB (copper chromium and boron salt). The analytical methods, such as flame atomic absorption spectrometry (FAAS), plasma inductively coupled optical emission spectrometry (ICPOES) and X-ray fluorescence spectrometry (XRFS) have been used for the analytical control of those treatment processes. In this work, the eucalyptus trees (Eucalyptus ssp) samples was obtained from Minas Gerais State, Brazil, cut plantation areas. Under pressure, eucalyptus wood samples were submitted to different concentration of CCA solution reaching 3.9, 6.7, 9.1, 12.4 and 14.0 kg of CCA by m-³ sapwood retentions. Samples in cylinders and sawdust forms were obtained from treated wood samples. Copper, chromium and arsenic determination was performed using the energy dispersive X-ray fluorescence spectrometry (EDXRFS), portable X-ray fluorescence spectrometry (PXRFS), flame atomic absorption spectrometry (FAAS) and instrumental neutron activation analysis. In this work, the method of analysis, sensitivity, precision and accuracy performances of the related techniques were outlined. (author)

Secondary-source energy-dispersive x-ray spectrometer

International Nuclear Information System (INIS)

Larsen, R.P.; Tisue, G.T.

1975-01-01

A secondary-source energy-dispersive x-ray spectrometer has been built and tested. In this instrument the primary source of x rays is a tungsten-target tube powered by a high-voltage (75 kV), a high-power (3.7 kW) generator from a wavelength spectrometer (G.E. XRD-6). The primary polychromatic x rays irradiate an elemental foil, the secondary source. Its characteristic essentially monochromatic x rays are used to irradiate the sample. Fluorescent x rays from the sample are detected and resolved by a lithium-drifted silicon detector, multichannel-analyzer system. The design of the instrument provides a convenient means for changing the secondary, and hence, the energy of the excitation radiation

Micro energy-dispersive x-ray fluorescence spectrometry study of dentin coating with nanobiomaterials

Science.gov (United States)

Soares, Luís. Eduardo Silva; Nahorny, Sídnei; Marciano, Fernanda Roberta; Zanin, Hudson; Lobo, Anderson de Oliveira

2015-06-01

New biomaterials such as multi-walled carbon nanotubes oxide/graphene oxide (MWCNTO/GO), nanohydroxyapatite (nHAp) and combination of them together or not to acidulated phosphate fluoride gel (F) have been tested as protective coating before root dentin erosion. Fourteen bovine teeth were cleaned, polished, divided into two parts (n=28) and assigned to seven groups: (Control) - without previous surface treatment; F treatment; nHAp; MWCNTO/GO; F+nHAp; F+MWCNTO/GO and F+MWCNTO/GO/nHAp composites. Each sample had two sites of pre-treatments: acid etched area and an area without treatment. After the biomaterials application, the samples were submitted to six cycles (demineralization: orange juice, 10 min; remineralization: artificial saliva, 1 h). Micro energy-dispersive X-ray fluorescence spectrometry (μ-EDXRF) mapping area analyses were performed after erosive cycling on both sites (n=84). μ-EDXRF mappings showed that artificial saliva and MWCNTO/GO/nHAp/F composite treatments produced lower dentin demineralization than in the other groups. Exposed dentin tubules allowed better interaction of nanobiomaterials than in smear layer covered dentin. Association of fluoride with other biomaterials had a positive influence on acid etched dentin. MWCNTO/GO/nHAp/F composite treatment resulted in levels of demineralization similar to the control group.

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

Science.gov (United States)

Palmer, Peter T.

2011-01-01

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

Optimization of a spectrometry for energy-dispersive x-ray fluorescence analysis by x-ray tube in combination with secondary target for multielements determination of sediment samples

International Nuclear Information System (INIS)

Zaidi Embong; Husin Wagiran

1997-01-01

The design of an energy-dispersive X-ray fluorescence spectrometer equipped with a conventional X-ray tube and secondary target is described. The spectrometer system constructed in our laboratory consists of a semiconductor detector system, irradiation chamber and X-ray tube. Primary source from X-ray tube was used to produced secondary X-ray from selenium, molybdenum and cadmium targets. The fluorescence X-ray from the sample was detected using Si(Li) detector with resolution of 0. 175 keV (Mn-K(x). The spectrometer was used for determination of multi-elements with atomic number between 20 to 44 in river sediment samples. The X-ray spectrum, from the samples were analysed using computer software which was developed based on Marquardt method. Optimal conditions and detection limits are determined experimentally by variation of excitation parameters for each combination of secondary target and tube voltage

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-07-01

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

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

International Nuclear Information System (INIS)

Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R.; Leite, Laudi C.; Lanna, Dante P.D.

2007-01-01

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

Dispersive liquid–liquid microextraction using diethyldithiocarbamate as a chelating agent and the dried-spot technique for the determination of Fe, Co, Ni, Cu, Zn, Se and Pb by energy-dispersive X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Kocot, Karina; Zawisza, Beata; Sitko, Rafal

2012-01-01

Dispersive liquid–liquid microextraction (DLLME) using sodium diethyldithiocarbamate (DDTC) as a chelating agent was investigated for the simultaneous determination of iron, cobalt, nickel, copper, zinc, selenium and lead ions in water samples. The procedure was performed using 5 mL of the sample, 100 μL of a 0.5% solution of DDTC, 30 μL of carbon tetrachloride (extraction phase) and 500 μL of methanol (disperser solvent). The experiments showed that Fe, Co, Ni, Cu, Zn and Pb can be simultaneously extracted at a pH of 5 and that Se can be extracted at a pH of 2–3. The results were compared with those obtained using ammonium pyrrolidine dithiocarbamate as a chelating agent. For all analytes, a linear range was observed up to 0.4 μg mL −1 . If Fe and Zn are present in concentrations 10 times higher than those of the other analytes, then the linearity is observed up to 0.2 μg mL −1 . In the present study, the organic phase that contained preconcentrated elements was deposited onto a Millipore filter and measured using energy-dispersive X-ray fluorescence spectrometry. The obtained detection limits were 2.9, 1.5, 2.0, 2.3, 2.5, 2.0 and 3.9 ng mL −1 for Fe, Co, Ni, Cu, Zn, Se and Pb, respectively. This combination of DLLME and the dried-spot technique is promising for multielement analyses using other spectroscopy techniques, such as laser ablation‐inductively coupled plasma‐mass spectrometry, laser-induced breakdown spectroscopy or total-reflection X-ray fluorescence spectrometry. - Highlights: ► Multielement trace analysis using dried-spot technique and dispersive liquid–liquid microextraction. ► Possibility of combination of LPME with EDXRF, LIBS or LA-ICP-MS. ► Comparison of APDC and DDTC as chelating agents.

X-ray spectrometry induced by electron and proton bombardment: Two complementary techniques for the micro-characterization of mineral materials

International Nuclear Information System (INIS)

Remond, G.; Gilles, C.; Isabelle, D.; Choi, C.G.; Rouer, O.; Cesbron, F.; Yang, C.

1994-01-01

Spatially resolved quantitative analysis by means of the Electron Probe Micro Analyser (EPMA) is now well established as a routine analytical method for point chemical analysis of a variety of mineral materials. Modern computer controlled EPMA are most often equipped with wavelength dispersive spectro- meters (WDS). Quantitative analyses are generally carried out according to a standard based approach, i. e, the x-ray intensities measured at the surface of the unknowns are normalized to those measured at the surface of reference specimens. By the use of energy dispersive spectrometry (EDS) a standardless quantitative based method is preferred when the incident beam current is not accurately known as for the case of EDS analysis coupled to Scanning Electron Microscopy (SEM). The accuracy of point analysis by means of electron beam induced x-ray spectrometry is discussed emphasizing the x-ray photon interactions respectively.The continuous x-ray emission is the physical limit of detection. The excitation conditions must be optimised in order to obtain the higher peak to continuous emission intensity ratios for each element within the matrix. Proton Induced X-ray Emission (PIXE) complements this electron induced x-ray emission for the localization of elements present at trace levels. The experimental procedure used for quantitative analysis by means of PIXE is illustrated emphasizing the use of a limited number of reference materials for deriving quantitative data from the raw PIXE spectra. The complementarity of EMPA/SEM and PIXE techniques is illustrated for the case of rare-earth elements (REE) bearing natural and synthetic doped zircon crystals (Si Zr O sub 4). For such compounds x-ray spectra are very complex because of the existence of severe peak overlaps between the L x-ray emission spectra of the REE. It is shown that cathodoluminescence (EPLA:SEM) and ionoluminescence (PIXE) may be an original alternative approach to x-ray spectrometry for studying REE

Trace and ultratrace determination of heavy metal ions by energy-dispersive X-ray fluorescence spectrometry using graphene as solid sorbent in dispersive micro solid-phase extraction

Energy Technology Data Exchange (ETDEWEB)

Kocot, Karina; Sitko, Rafal, E-mail: rafal.sitko@us.edu.pl

2014-04-01

In this paper, the adsorptive properties of graphene nanosheets were used for simultaneous preconcentration of cobalt, nickel, copper and lead ions from water samples. The developed methodology is based on dispersive micro-solid phase extraction (DMSPE) which is miniaturized and a simplified version of classical solid phase extraction technique. In proposed procedure only 200 μL of suspension containing graphene (0.2 mg), ammonium pyrrolidine dithiocarbamate (APDC) (0.8 mg) and Triton-X-100 (0.1 mg) is rapidly injected to 50 mL of water sample. Then, graphene nanosheets with adsorbed metal-APDC chelates are collected on membrane filter and measured using energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The various parameters including pH, amount of APDC, sample volume, amount of Triton-X-100 and sorption time were optimized in order to obtain the best recoveries. The experiment shows that Co, Ni, Cu and Pb can be simultaneously preconcentrated at pH of 5 with high recoveries (97%, 96%, 99% and 96% for Co, Ni, Cu and Pb, respectively) and very good precision (RSDs within 2.6–3.4%). Due to the excellent enrichment factors ranging from 400 to 2500 the proposed DMSPE–EDXRF procedure offers low detection limits. For optimized measurement conditions (voltage and current of X-ray tube, primary beam filter) the detection limits are even 0.08, 0.07, 0.08 and 0.20 ng mL{sup −1} for Co, Ni, Cu and Pb, respectively. - Highlights: • Excellent detection limits using EDXRF • A new preconcentration procedure combining DMSPE and EDXRF measurement • Graphene as a promising and efficient solid sorbent in DMSPE • Simple, fast, inexpensive and environmental friendly method.

X-ray fluorescence imaging with polycapillary X-ray optics

International Nuclear Information System (INIS)

Yonehara, Tasuku; Yamaguchi, Makoto; Tsuji, Kouichi

2010-01-01

X-ray fluorescence spectrometry imaging is a powerful tool to provide information about the chemical composition and elemental distribution of a specimen. X-ray fluorescence spectrometry images were conventionally obtained by using a μ-X-ray fluorescence spectrometry spectrometer, which requires scanning a sample. Faster X-ray fluorescence spectrometry imaging would be achieved by eliminating the process of sample scanning. Thus, we developed an X-ray fluorescence spectrometry imaging instrument without sample scanning by using polycapillary X-ray optics, which had energy filter characteristics caused by the energy dependence of the total reflection phenomenon. In the present paper, we show that two independent straight polycapillary X-ray optics could be used as an energy filter of X-rays for X-ray fluorescence. Only low energy X-rays were detected when the angle between the two optical axes was increased slightly. Energy-selective X-ray fluorescence spectrometry images with projection mode were taken by using an X-ray CCD camera equipped with two polycapillary optics. It was shown that Fe Kα (6.40 keV) and Cu Kα (8.04 keV) could be discriminated for Fe and Cu foils.

A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

Science.gov (United States)

Rathi, Monika; Ahrenkiel, S P; Carapella, J J; Wanlass, M W

2013-02-01

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy-based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

X-ray fluorescence and gamma-ray spectrometry combined with multivariate analysis for topographic studies in agricultural soil

International Nuclear Information System (INIS)

Castilhos, Natara D.B. de; Melquiades, Fábio L.; Thomaz, Edivaldo L.; Bastos, Rodrigo Oliveira

2015-01-01

Physical and chemical properties of soils play a major role in the evaluation of different geochemical signature, soil quality, discrimination of land use type, soil provenance and soil degradation. The objectives of the present study are the soil elemental characterization and soil differentiation in topographic sequence and depth, using Energy Dispersive X-Ray Fluorescence (EDXRF) as well as gamma-ray spectrometry data combined with Principal Component Analysis (PCA). The study area is an agricultural region of Boa Vista catchment which is located at Guamiranga municipality, Brazil. PCA analysis was performed with four different data sets: spectral data from EDXRF, spectral data from gamma-ray spectrometry, concentration values from EDXRF measurements and concentration values from gamma-ray spectrometry. All PCAs showed similar results, confirmed by hierarchical cluster analysis, allowing the data grouping into top, bottom and riparian zone samples, i.e. the samples were separated due to its landscape position. The two hillslopes present the same behavior independent of the land use history. There are distinctive and characteristic patterns in the analyzed soil. The methodologies presented are promising and could be used to infer significant information about the region to be studied. - Highlights: • Characterization of topographic sequence of two hillslopes from agricultural soil. • Employment of EDXRF and gamma-ray spectrometry data combined with PCA. • The combination of green analytical methodologies with chemometric studies allowed soil differentiation. • The innovative methodology is promising for direct characterization of agricultural catchments

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

African Journals Online (AJOL)

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

X-ray energy-dispersive diffractometry using synchrotron radiation

International Nuclear Information System (INIS)

Buras, B.; Staun Olsen, J.; Gerward, L.

1977-03-01

In contrast to bremsstrahlung from X-ray tubes, synchrotron radiation is very intense, has a smooth spectrum, its polarization is well defined, and at DESY the range of useful photon energies can be extended to about 70 keV and higher. In addition the X-ray beam is very well collimated. Thus synchrotron radiation seems to be an ideal X-ray source for energy-dispersive diffractometry. This note briefly describes the experimental set up at DESY, shows examples of results, and presents the underlying 'philosophy' of the research programme. (Auth.)

Analysis of Precious Stones Deposited in Various Rock Samples of Mogok Region by energy dispersive X-ray Fluorescence Spectrometry

International Nuclear Information System (INIS)

Kyi Kyi San; Soe Lwin; Win Win Thar; Sein Htoon

2004-06-01

The analysis of precious stones deposited in various rock samples of Mogok region were investigated by the energy dispersive x-ray fluorescence technique. The x-ray machine with Rh target was used to excite the characteristic x-ray from the sample. X-rays emitted from the sample were measured by a high resolution, cooled Si (Li) detector. The calibration was made by the measurement of minerals which composed in each kind of precious stones. The kind of precious stone deposited in the rocks sample was determined by the measurement of minerals from the rock samples compared with those obtained from each kind of precious stones

Quantitative analysis with energy dispersive X-ray fluorescence analyser

International Nuclear Information System (INIS)

Kataria, S.K.; Kapoor, S.S.; Lal, M.; Rao, B.V.N.

1977-01-01

Quantitative analysis of samples using radioisotope excited energy dispersive x-ray fluorescence system is described. The complete set-up is built around a locally made Si(Li) detector x-ray spectrometer with an energy resolution of 220 eV at 5.94 KeV. The photopeaks observed in the x-ray fluorescence spectra are fitted with a Gaussian function and the intensities of the characteristic x-ray lines are extracted, which in turn are used for calculating the elemental concentrations. The results for a few typical cases are presented. (author)

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

International Nuclear Information System (INIS)

Almeida, Eduardo de; Senicato, Luis A; Nascimento Filho, Virgilio F.; Gomide, Catarina A.

2007-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-07-01

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

Forensic application of total reflection X-ray fluorescence spectrometry for elemental characterization of ink samples

International Nuclear Information System (INIS)

Dhara, Sangita; Misra, N.L.; Maind, S.D.; Kumar, Sanjukta A.; Chattopadhyay, N.; Aggarwal, S.K.

2010-01-01

The possibility of applying Total Reflection X-ray Fluorescence for qualitative and quantitative differentiation of documents printed with rare earth tagged and untagged inks has been explored in this paper. For qualitative differentiation, a very small amount of ink was loosened from the printed documents by smoothly rubbing with a new clean blade without destroying the manuscript. 50 μL of Milli-Q water was put on this loose powder, on the manuscript, and was agitated by sucking and releasing the suspension two to three times with the help of a micropipette. The resultant dispersion was deposited on quartz sample support for Total Reflection X-ray Fluorescence measurements. The Total Reflection X-ray Fluorescence spectrum of tagged and untagged inks could be clearly differentiated. In order to see the applicability of Total Reflection X-ray Fluorescence for quantitative determinations of rare earths and also to countercheck such determinations in ink samples, the amounts of rare earth in painted papers with single rare earth tagged inks were determined by digesting the painted paper in HNO 3 /HClO 4 , mixing this solution with the internal standard and recording their Total Reflection X-ray Fluorescence spectra after calibration of the instrument. The results thus obtained were compared with those obtained by Inductively Coupled Plasma Mass Spectrometry and were found in good agreement. The average precision of the Total Reflection X-ray Fluorescence determinations was 5.5% (1σ) and the average deviation of Total Reflection X-ray Fluorescence determined values with that of Inductively Coupled Plasma Mass Spectrometry was 7.3%. These studies have shown that Total Reflection X-ray Fluorescence offers a promising and potential application in forensic work of this nature.

Forensic application of total reflection X-ray fluorescence spectrometry for elemental characterization of ink samples

Energy Technology Data Exchange (ETDEWEB)

Dhara, Sangita [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Misra, N.L., E-mail: nlmisra@barc.gov.i [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Maind, S.D. [NAA Unit of Central Forensic Science Laboratory Hyderabad at Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Kumar, Sanjukta A. [Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Chattopadhyay, N. [NAA Unit of Central Forensic Science Laboratory Hyderabad at Analytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Aggarwal, S.K. [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India)

2010-02-15

The possibility of applying Total Reflection X-ray Fluorescence for qualitative and quantitative differentiation of documents printed with rare earth tagged and untagged inks has been explored in this paper. For qualitative differentiation, a very small amount of ink was loosened from the printed documents by smoothly rubbing with a new clean blade without destroying the manuscript. 50 muL of Milli-Q water was put on this loose powder, on the manuscript, and was agitated by sucking and releasing the suspension two to three times with the help of a micropipette. The resultant dispersion was deposited on quartz sample support for Total Reflection X-ray Fluorescence measurements. The Total Reflection X-ray Fluorescence spectrum of tagged and untagged inks could be clearly differentiated. In order to see the applicability of Total Reflection X-ray Fluorescence for quantitative determinations of rare earths and also to countercheck such determinations in ink samples, the amounts of rare earth in painted papers with single rare earth tagged inks were determined by digesting the painted paper in HNO{sub 3}/HClO{sub 4}, mixing this solution with the internal standard and recording their Total Reflection X-ray Fluorescence spectra after calibration of the instrument. The results thus obtained were compared with those obtained by Inductively Coupled Plasma Mass Spectrometry and were found in good agreement. The average precision of the Total Reflection X-ray Fluorescence determinations was 5.5% (1sigma) and the average deviation of Total Reflection X-ray Fluorescence determined values with that of Inductively Coupled Plasma Mass Spectrometry was 7.3%. These studies have shown that Total Reflection X-ray Fluorescence offers a promising and potential application in forensic work of this nature.

X-ray fluorescence spectrometers: a comparison of wavelength and energy dispersive instruments

International Nuclear Information System (INIS)

Slates, R.V.

1977-11-01

Wavelength dispersive and energy dispersive x-ray fluorescence spectrometers are compared. Separate sections are devoted to principles of operation, sample excitation, spectral resolution, and x-ray detection. Tabulated data from the literature are cited in the comparison of accuracy, precision, and detection limits. Spectral interferences and distortions are discussed. Advantages and limitations are listed for simultaneous wavelength dispersive spectrometers, sequential wavelength dispersive spectrometers, and Si(Li) energy dispersive spectrometers. Accuracy, precision, and detection limits are generally superior for wavelength dispersive spectrometers

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

Science.gov (United States)

Ohata, Masaki; Kidokoro, Toshihiro; Hioki, Akiharu

2012-01-01

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

Development of a portable system of X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Mantuano, Andrea; Crisostomo, Jose V.V.; Barros, Mariana J.; Oliveira, Luis F.; Barroso, Regina C.

2009-01-01

This paper develops a compact and portable spectrometry system that will be used at the Laboratory of Applied Physics to the Biomedical and Environmental Sciences of the Institute of Physics/UERJ, Rio de Janeiro, Brazil. The laboratory both prepares the samples and develops the X-ray spectrometry techniques. The techniques of X-ray diffraction and fluorescence on various samples (biological, industrial and environmental) are used, attending to pos-graduation and graduation students, with multidisciplinary characteristics. The Mini-X system consists of X-ray mini tube MINI-X from Amptek with tungsten (W) target, and a compact spectrometer X123, also from Amptek that includes a detector, pre-amplifier, digital pulse processor, and multichannel. All the system is controlled by dedicated microprocessor. This work will present both a methodology for alignment and calibration of the system as far the first measurements performed using the X-ray fluorescence technique on standard samples. The multi elementary analysis by X-ray fluorescence (XRF) is based on the measurements of the characteristic X-ray intensity emitted by the chemical elements components of the samples when excited. Therefore, from the development of this compact and versatile system it will be possible to obtain the fluorescent intensities of the analysed samples at the Laboratory, not only at the research area but at the teaching area. Besides, new laboratory practices are being developed for the discipline of medical physics

X-ray analysis and mapping by wavelength dispersive X-ray spectroscopy in an electron microscope

International Nuclear Information System (INIS)

Tanaka, Miyoko; Takeguchi, Masaki; Furuya, Kazuo

2008-01-01

A compact and easy-to-use wavelength dispersive X-ray spectrometer using a multi-capillary X-ray lens attached to a scanning (transmission) electron microscope has been tested for thin-film analysis. B-K spectra from thin-film boron compounds (B 4 C, h-BN, and B 2 O 3 ) samples showed prominent peak shifts and detailed structural differences. Mapping images of a thin W/Si double-layer sample resolved each element clearly. Additionally, a thin SiO 2 film grown on a Si substrate was imaged with O-K X-rays. Energy and spatial resolution of the system is also discussed

Angle-resolved X-ray fluorescence spectrometry using synchrotron radiation at ELSA

International Nuclear Information System (INIS)

Schmitt, W.; Rothe, J.; Hormes, J.; Gries, W.H.

1994-01-01

Measurements on the centroid depth of ion-implanted phosphorus-in-silicon specimen by the method of angle-resolved, self-ratio X-ray fluorescence spectrometry (AR/SR/XFS) have been carried out using 'white' synchrotron radiation (SR). The measurements were performed using a modified wavelength-dispersive fluorescence spectrometer. Problems due to the use of SR, like carbonaceous specimen contamination and sample heating were overcome by flooding the specimen chamber with helium and by pre-absorbing the non-exciting parts of the incident SR with suitable filters, respectively. The decaying primary intensity was monitored by measuring the compensation current of the photoelectrons emitted from a tungsten wire stretched across the primary beam. Results have been obtained for specimen with dose density levels of 10 16 cm -2 and 3x10 15 cm -2 . (orig.)

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

DEFF Research Database (Denmark)

Kunzendorf, Helmar; Wollenberg, H.A.

1970-01-01

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

use of x-ray fluorescence spectrometry to determine trace elements ...

African Journals Online (AJOL)

NIJOTECH

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

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

African Journals Online (AJOL)

Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

Scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and aerosol time-of-flight mass spectrometry (ATOFMS) single particle analysis of metallurgy plant emissions.

Science.gov (United States)

Arndt, J; Deboudt, K; Anderson, A; Blondel, A; Eliet, S; Flament, P; Fourmentin, M; Healy, R M; Savary, V; Setyan, A; Wenger, J C

2016-03-01

The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe-Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of lead associated with airborne particulate matter by flame atomic absorption and wave-length dispersive x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Talebi, S.M.

1997-01-01

The lead content of airborne particulate matter was determined by flame atomic absorption spectrometry (FAAS) following digestion with a mixture of nitric acid and hydrogen peroxide and also by wave-length dispersive x-ray fluorescence (WDXRF). The extraction procedure was checked by analyzing a standard reference material of airborne particulate matter (NIST, SRM -1648). It was concluded that lead can quantitatively (98%) be extracted from airborne particulate matter by the leaching process. A five-stage sequential extraction was performed to assess the potential mobility of lead associated with airborne particulate matter. Comparison of the airborne particulate lead measured by WDXRF to that measured by FAAS showed good agreement. The WDXRF method requires no time-consuming sample preparation or use of environmentally unfriendly solvents. The technique is suggested for direct determination of lead in airborne particulate matter in air pollution studies. (author)

X-ray fluorescence spectrometry - an introduction course

International Nuclear Information System (INIS)

Salvador, V.L.R.

1989-01-01

The theoretical and experimental principles of the X-ray fluorescence spectrometry, is presented the text is a synthesis of the most important literature in this area. The authors included are: E.P. Bertin, R. Jenkins, J.L. Devries, R. Muller, R. Tertian, F. Claisse e K.L. Willians. (author)

The application of X-ray fluorescence spectrometry to prospecting potential gold deposits

International Nuclear Information System (INIS)

Shang Fengjun; Wang Haixia; Zhou Rongsheng

2001-01-01

The fieldwork high-sensitivity X-ray fluorescence analysis (FXFA) adopting miniaturized X-ray tube, Si-PIN detector with peltier cooler and notebook PC spectrometry is presented. Using this system, the authors carried out a preliminary research of its application to some gold mine in Sichuan. According to the close relationship between the high-grade element arsenic and gold in ore-forming components, X-ray fluorescence spectrometry can be used to reveal the existence of potential gold mineralization in fields rapidly. This is of great significance in guiding the field geological collection

Instrumental aspects of tube-excited energy-dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Adams, F.; Nullens, H.; Espen, P. van

1983-01-01

Energy-dispersive X-ray fluorescence spectrometry is an attractive and widely used method for sensitive multi-element analysis. The method suffers from the extreme density of spectral components in a rather limited energy range which implies the need for computer based spectrum analysis. The method of iterative least squares analysis is the most powerful tool for this. It requires a systematic and accurate description of the spectral features. Other important necessities for accurate analysis are the calibration of the spectrometer and the correction for matrix absorption effects in the sample; they can be calculated from available physical constants. Ours and similar procedures prove that semi-automatic analyses are possible with an accuracy of the order of 5%. (author)

A low power x-ray tube for use in energy dispersive x-ray fluorescence analysis

International Nuclear Information System (INIS)

Kataria, S.K.; Govil, Rekha; Lal, M.

1980-01-01

A low power X-ray tube with thin molybdenum transmission target for use in energy dispersive X-ray fluorescence (ENDXRF) element analysis has been indigenously built, along with its power supply. The X-ray tube has been in operation since August 1979, and it has been operated upto maximum target voltage of 35 KV and tube current upto 200 μA which is more than sufficient for trace element analysis. This X-ray tube has been used alongwith the indigenously built Si(Li) detector X-ray spectrometer with an energy resolution of 200 eV at 5.9 Kev MnKsub(α) X-ray peak for ENDXRF analysis. A simple procedure of calibration has been developed for thin samples based on the cellulose diluted, thin multielement standard pellets. Analytical sensitivities of the order of a few p.p.m. have been obtained with the experimental setup for elements with 20 < = Z < = 38 and 60 < = Z < = 90. A number of X-ray spectra for samples of environmental, biological, agricultural, industrial and metallurgical interest are presented to demonstrate the salient features of the experimental sep up. (auth.)

Compilation of monographs on α-, β-, γ- and X-ray spectrometry

International Nuclear Information System (INIS)

Debertin, K.

1977-11-01

The working group 'α-, β-, γ-Ray Spectrometry' of the International Committee for Radionuclide Metrology (ICRM) compiled about 35 monographs on α-, β-, γ- and X-ray spectrometry which were published in the years 1970 to 1976. Support was obtained by the Zentralstelle fuer Atomkernenergie-Dokumentation (ZAED) in Karlsruhe. (orig.) [de

X-ray chemical analyzer for field applications

International Nuclear Information System (INIS)

Gamba, O.O.M.

1977-01-01

A self-supporting portable field multichannel x-ray chemical analyzer system is claimed. It comprises a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an x-ray energy dispersive spectrometry technique

Application of energy dispersive X-ray fluorescence spectrometry to polychrome terracotta sculptures from the Alcobaça Monastery, Portugal

Directory of Open Access Journals (Sweden)

Agnès Le Gac

2014-01-01

Full Text Available Portable energy dispersive X-ray fluorescence spectrometry (EDXRF was used in the Alcobaça Monastery, in order to study the chromatic coatings applied to terracotta statues that belong to two seventeenth-century monumental groupings. The main goal of this scientific approach consisted in determining the elemental composition of the constitutive layers and in trying to reconstitute the existing polychromy, taking into account the technical aspects observed at naked eye. The measurements carried out by EDXRF allowed a first material characterization of these artworks. By comparing the results obtained in each statue, it was possible to attest the application of a seventeenth-century coating to each one and at least a subsequent intervention in the form of a refurbishment or a new polychromy. According to the materials employed in their production, it appears that the refurbishment is likely dated from the 19th century while the new polychromy is still dated from the 18th century.

Wave-dispersive x-ray spectrometer for simultaneous acquisition of several characteristic lines based on strongly and accurately shaped Ge crystal

International Nuclear Information System (INIS)

Hayashi, Kouichi; Nakajima, Kazuo; Fujiwara, Kozo; Nishikata, Susumu

2008-01-01

Si and Ge are widely used as analyzing crystals for x-rays. Drastic and accurate shaping of Si or Ge gives significant advance in the x-ray field, although covalently bonded Si or Ge crystals have long been believed to be not deformable to various shapes. Recently, we developed a deformation technique for obtaining strongly and accurately shaped Si or Ge wafers of high crystal quality, and the use of the deformed wafer made it possible to produce fine-focused x-rays. In the present study, we prepared a cylindrical Ge wafer with a radius of curvature of 50 mm, and acquired fluorescent x-rays simultaneously from four elements by combining the cylindrical Ge wafer with a position-sensitive detector. The energy resolution of the x-ray fluorescence spectrum was as good as that obtained using a flat single crystal, and its gain was over 100. The demonstration of the simultaneous acquisition of high-resolution x-ray fluorescence spectra indicated various possibilities of x-ray spectrometry, such as one-shot x-ray spectroscopy and highly efficient wave-dispersive x-ray spectrometers

The dispersion surface of X-rays very near the absorption edge

International Nuclear Information System (INIS)

Fukamachi, T.; Negishi, R.; Kawamura, T.

1995-01-01

To discuss the X-ray dynamical diffraction when the imaginary part of the X-ray polarizability is larger than the real part, the dispersion surface is studied as a function of the ratio between the real and the imaginary parts of the polarizability. The dispersion surface in the Laue case when the real part is zero has a similar form to that in the Bragg case when the imaginary part is zero. The relations between the dispersion surface and the diffracted intensity are studied in some special cases. The abnormal absorption and the abnormal transmission effect are related to the features of the dispersion surface. (orig.)

Energy-dispersive X-ray fluorescence analysis of organic-rich soils and sediments

International Nuclear Information System (INIS)

Parekh, P.P.

1981-01-01

A method has been developed for elemental analysis of environmental samples of soils and sediments rich in organic matter by energy-dispersive X-ray fluorescence spectrometry. It consists of three steps (i) determining the apparent concentration of elements by using calibration coefficients based on geochemical standards, (ii) subsequent assay of the total organic matter (TOM) from loss on ignition at 550 deg C, and (iii) evaluating the correct elemental concentration by normalizing for transparency from an empirical relationship. The main feature of the method is the sample analysis prior to ignition, which avoids any loss of trace elements - especially the volatile toxic elements, such as Zn, As, Se, and Pb - during heating. The method was tested on two organic-rich lake sediments (TOM> 30%). Concentrations of five elements (K, Mn, Fe, Zn, and Pb) determined by the present method and by atomic absorption spectrometry agreed within about +-10%. (author)

Characterization of chemical elements in soil submitted to different systems use and management by energy dispersive x-ray fluorescence spectrometry (EDXRF)

International Nuclear Information System (INIS)

Wastowski, Arci Dirceu; Rosa, Genesio Mario da; Cherubin, Mauricio Roberto; Rigon, Joao Paulo Gonsiorkiewicz

2010-01-01

This study aimed to evaluate the chemical elements levels in soil, submitted to different management systems and use by the Energy Dispersive X-Ray Fluorescence Spectrometry - EDXRF. The systems were T1 - agroforestry (SAF), T2 - native field (CN), T3 - native forest (NM), T4 - tillage forest (PF); T5 - conventional tillage system (SPC) and T6 - system tillage (NT). Samples were collected at 0-10 and 10-20 cm, dried and ground for analysis in EDX-720. The soil showed no difference in the average concentrations of chemical elements analyzed in the profiles, but the systems presented different concentrations of metal elements, and T3 had the highest K, Ca and Zn at 0-10 cm and higher contents of K, Ca, Cu, Zn and Mn in the layer of 10-20 cm. (author)

Target characterization by PIXE, alpha spectrometry and X-ray absorption

International Nuclear Information System (INIS)

Kheswa, N.Y.; Papka, P.; Pineda-Vargas, C.A.; Newman, R.T.

2011-01-01

We report on the thickness and homogeneity characterization of thin metallic targets of Zr-96 by means of alpha absorption spectrometry, Particle Induced X-ray Emission (PIXE) and X-ray absorption. The target thicknesses determined by means of the above mentioned methods are critically compared. The thicknesses were determined before and after irradiation with a 70 MeV beam of 14 N ions.

Determination of chlorine in coal by X-ray fluorescence spectrometry method

Energy Technology Data Exchange (ETDEWEB)

Marek, S.; Bojarska, K. [Central Mining Institute, Katowice (Poland). Dept. of Environmental Monitoring

1997-12-31

Determination of chlorine contents in coal is essential for both environmental protection and its technological use. The existing method of chlorine determination in coal are titration methods which have considerable errors particularly in the low concentration range. The elaborated method with the use of X-ray fluorescence spectrometry in a comparison to the other methods is much faster and has better precision and accuracy. The principle of the method lies in the measurement of X-ray fluorescence radiation intensity which is emitted by chlorine in a sample and its comparison with standards. The calibration of the elaborated XRF method is based on natural coals having various concentrations of chlorine within the whole range of its occurrence in Polish coals. Concentrations for the calibration purpose were obtained by the determination of chlorine contents in selected coals by atomic absorption spectrometry method. The procedure of sample preparation for direct X-ray measurements, instrumental measuring conditions and the way of calibration curve preparation are described in the paper. All X-ray measurements were done with a Phillips sequential X-ray fluorescence spectrometer. A double anode Cr-Au X-ray tube with maximum power 3000 MW was used as the excitation source. 5 figs., 4 tabs.

Handbook of X-Ray Data

CERN Document Server

Zschornack, Günter

2007-01-01

This sourcebook is intended as an X-ray data reference for scientists and engineers working in the field of energy or wavelength dispersive X-ray spectrometry and related fields of basic and applied research, technology, or process and quality controlling. In a concise and informative manner, the most important data connected with the emission of characteristic X-ray lines are tabulated for all elements up to Z = 95 (Americium). This includes X-ray energies, emission rates and widths as well as level characteristics such as binding energies, fluorescence yields, level widths and absorption edges. The tabulated data are characterized and, in most cases, evaluated. Furthermore, all important processes and phenomena connected with the production, emission and detection of characteristic X-rays are discussed. This reference book addresses all researchers and practitioners working with X-ray radiation and fills a gap in the available literature.

Energy dispersive X-ray spectroscopy with microcalorimeters

International Nuclear Information System (INIS)

Hollerith, C.; Wernicke, D.; Buehler, M.; Feilitzsch, F. von; Huber, M.; Hoehne, J.; Hertrich, T.; Jochum, J.; Phelan, K.; Stark, M.; Simmnacher, B.; Weiland, W.; Westphal, W.

2004-01-01

Shrinking feature sizes in semiconductor device production as well as the use of new materials demand innovation in device technology and material analysis. X-ray spectrometers based on superconducting sensor technology are currently closing the gap between fast energy dispersive spectroscopy (EDS) and high-resolution wavelength dispersive spectroscopy (WDS). This work reports on the successful integration of iridium/gold transition edge sensors in the first industrially used microcalorimeter EDS. The POLARIS microcalorimeter system is installed at the failure analysis lab FA5 at Infineon Technologies AG in Neuperlach (Munich) and is used in routine analysis

X-ray fluorescence spectrometry used to assess the dispersion of metals within mining environments; Aplicacion de la tecnica de espectrometria de fluorescencia de rayos-X en el estudio de la dispersion de metales en areas mineras

Energy Technology Data Exchange (ETDEWEB)

Margui, E.; Gonzalez-Fernandez, O.; Hidalgo, M.; Pardini, G.; Queralt, I.

2011-07-01

One critical factor for success in characterizing metals polluting mining environments so as to be able to eliminate them and subsequently recover these areas depends upon a speedy and correct response in the analysis of samples. Rapid, simultaneous, multi-element analysis can be undertaken using X-ray fluorescence spectrometry, a versatile, non-destructive analytical technique commonly employed to identify both major and minor elements in samples related to environmental studies. An additional advantage of this technique is the possibility of conducting the analysis directly on solid samples, which is extremely convenient when dealing with environmental samples that are difficult to dissolve, such as soils, sediments and mining wastes. Moreover, in recent years the development of spectrometers equipped with digital-signal processors combined with enlarged X-ray production, using better designs for excitation-detection, has contributed to an improvement in instrumental sensitivity, thus allowing us to detect important polluting elements such as Cd and Pb at trace levels. In this paper the authors describe, on the basis of their own experience, some interesting applications of XRF spectrometry for the analysis of several types of environmental samples related to the study of the dispersion of metals within mining environments: (A) analysis of mining wastes, soils and sediments; (B) analysis of samples of vegetation used as bio indicators or related to phyto remediation studies; and (C) analysis of water samples related to mining operations. (Author) 26 refs.

Determination of inorganic nutrients in wheat flour by laser-induced breakdown spectroscopy and energy dispersive X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Peruchi, Lidiane Cristina; Nunes, Lidiane Cristina; Gustinelli Arantes de Carvalho, Gabriel; Guerra, Marcelo Braga Bueno; Almeida, Eduardo de; Rufini, Iolanda Aparecida [NAPTISA Research Support Center “Technology and Innovation for a Sustainable Agriculture”, Center for Nuclear Energy in Agriculture, University of São Paulo, Av. Centenário 303, 13416-000, Piracicaba SP (Brazil); Santos, Dário [Federal University of São Paulo, R. Prof. Artur Riedel 275, 09972-270, Diadema SP (Brazil); Krug, Francisco José, E-mail: fjkrug@cena.usp.br [NAPTISA Research Support Center “Technology and Innovation for a Sustainable Agriculture”, Center for Nuclear Energy in Agriculture, University of São Paulo, Av. Centenário 303, 13416-000, Piracicaba SP (Brazil)

2014-10-01

Laser-induced breakdown spectroscopy (LIBS) and energy dispersive X-ray fluorescence spectrometry (EDXRF) were evaluated for the determination of P, K, Ca, Mg, S, Fe, Cu, Mn and Zn in pressed pellets of wheat flours. EDXRF and LIBS calibration models were built with analytes mass fractions determined by inductively coupled plasma optical emission spectrometry after microwave-assisted acid digestion in a set of 25 wheat flour laboratory samples. Test samples consisted of pressed pellets prepared from wheat flour mixed with 30% mm{sup −1} cellulose binder. Experiments were carried out with a LIBS setup consisted of a Q-switched Nd:YAG laser and a spectrometer with Echelle optics and ICCD, and a benchtop EDXRF system fitted with a Rh target X-ray tube and a Si(Li) semiconductor detector. The correlation coefficients from the linear calibration models of P, K, Ca, Mg, S, Fe, Mn and Zn determined by LIBS and/or EDXRF varied from 0.9705 for Zn to 0.9990 for Mg by LIBS, and from 0.9306 for S to 0.9974 for K by EDXRF. The coefficients of variation of measurements varied from 1.2 to 20% for LIBS, and from 0.3 to 24% for EDXRF. The predictive capabilities based on RMSEP (root mean square error of prediction) values were appropriate for the determination of P, Ca, Mg, Fe, Mn and Zn by LIBS, and for P, K, S, Ca, Fe, and Zn by EDXRF. In general, results from the analysis of NIST SRM 1567a Wheat flour by LIBS and EDXRF were in agreement with their certified mass fractions. - Highlights: • Combination of LIBS and EDXRF for quantitative analysis of wheat flour. • Validation performed for determination of P, K, Ca, Mg, S, Fe, Cu, Mn and Zn. • Same test samples can be used for both methods. • Appropriate limits of detection for all tested analytes. • Methods are simple and provide fast and accurate results for routine analysis.

Compact energy dispersive X-ray microdiffractometer for diagnosis of neoplastic tissues

Science.gov (United States)

Sosa, C.; Malezan, A.; Poletti, M. E.; Perez, R. D.

2017-08-01

An energy dispersive X-ray microdiffractometer with capillary optics has been developed for characterizing breast cancer. The employment of low divergence capillary optics helps to reduce the setup size to a few centimeters, while providing a lateral spatial resolution of 100 μm. The system angular calibration and momentum transfer resolution were assessed by a detailed study of a polycrystalline reference material. The performance of the system was tested by means of the analysis of tissue-equivalent samples previously characterized by conventional X-ray diffraction. In addition, a simplified correction model for an appropriate comparison of the diffraction spectra was developed and validated. Finally, the system was employed to evaluate normal and neoplastic human breast samples, in order to determine their X-ray scatter signatures. The initial results indicate that the use of this compact energy dispersive X-ray microdiffractometer combined with a simplified correction procedure is able to provide additional information to breast cancer diagnosis.

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

African Journals Online (AJOL)

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

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

Science.gov (United States)

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

2010-12-28

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

Installation for β- and X-ray spectrometry

International Nuclear Information System (INIS)

Sokolov, A.D.; Pchelintsev, A.B.; Lupilov, A.V.; Zalinkevich, V.A.; Lapenas, A.

2002-01-01

Paper presents design and parameters of an installation for spectrometry of β- particles and conversion electrons within 15-3000 keV energy range and for X-ray radiation within 2-60 keV range. Si(Li) detector with 500 mm 2 area and 4.5 mm sensitive range thickness is used to record radiation. Energy resolution for 624 keV energy conversion electrons constitutes [ru

Assembly of positioner of automated two-dimensional scan coupled to X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Silva, Leonardo Santiago Melgaço

2011-01-01

This work describes the design and assembling of a prototype automated positioner two-dimensional scanning coupled to X-ray fluorescence spectrometry. The work aims to achieve a portable and easy to use, device of broad utility in the analysis of samples by X-ray fluorescence area of expertise and research. The two-dimensional scanning of the positioner is by means of two stepper motors controlled by a microcontroller PIC 16F877A, encoder and optical sensors. The user interacts with the XY table through an interface program for the Windows operating system, which communicates with the microcontroller through the serial port. The system of Fluorescence Spectroscopy incorporated into the positioner consists of a system commercially available system from the company AMPTEK, where the primary source of excitation of the sample was a source of 241 Am of 59.5 KeV emissions. Resolution and accuracy of tests were performed in the XY scanning process and reproducibility of the same kit with the fluorescence spectrometry X-ray. Qualitative tests by X-ray fluorescence spectrometry in samples were performed to demonstrate the applicability and versatility of the project. It follows that the prototype illustrates a possible adequately to portable device for X-ray spectrometry of two-dimensional. (author)

Determination of 239Pu and 240Pu isotope ratio for a nuclear bomb particle using X-ray spectrometry in conjunction with γ-ray spectrometry and non-destructive α-particle spectrometry

International Nuclear Information System (INIS)

Poellaenen, R.; Ruotsalainen, K.; Toivonen, H.

2009-01-01

A nuclear bomb particle from Thule containing Pu and U was analyzed using X-ray spectrometry in combination with γ-ray spectrometry and non-destructive α-spectrometry. The main objective was to investigate the possibility to determine the 239 Pu and 240 Pu isotope ratios. Previously, X-ray spectrometry together with the above-mentioned methods has been successfully applied for radiochemically processed samples, but not for individual particles. In the present paper we demonstrate the power of non-destructive analysis. The 239 Pu/( 239 Pu+ 240 Pu) atom ratio for the Thule particle was determined, using two different approaches, to be 0.93±0.07 and 0.91±0.05. These results are consistent with weapons-grade material and the results obtained by other investigators.

A strategy for vitrification product assurance and control with X-ray fluorescence spectrometry (PACX)

International Nuclear Information System (INIS)

Resce, J.L.

1995-01-01

A product control strategy is proposed for the vitrification of low-level and/or mixed waste. This strategy is called Product Assurance and Control with X-ray fluorescence spectrometry (PACX). The strategy utilizes sequential wavelength dispersive x-ray fluorescence spectrometry and standardless fundamental parameters calculations to analyze both the melter feed and the glassy products. The melter feed is sampled prior to addition to the melt tank and then melted and cast into samples which should closely resemble the product from the vitrification process itself. The resulting sample disks are then analyzed by x-ray fluorescence spectrometry. All elements with atomic numbers down to sodium can be determined directly and then either boron or lithium can be determined by difference from the mass balance. The XRF intensities are converted into oxide compositions with the use of a novel standardless fundamental parameters program. Previous work has shown that there is an excellent correlation between the XRF results and the results from conventional wet chemical analyses, but the XRF results can be obtained within two to three hours of sampling. If compositional control limits for durability are available, the product acceptability can be determined prior to the batch being introduced into the melter. The durability could also be estimated from a model, if available, which predicts product durability from composition. If the predicted durability is estimated to be too low, the model can then be used to determine additives which will raise the durability of the final product to within acceptable limits. The additives can then be incorporated into the batch prior to addition into the melter. A similar XRF analysis can be carried out on the glass product from the melter which can then be used to predict and thus assure product acceptance

Measuring conditions for second order X-ray Bragg-spectrometry

International Nuclear Information System (INIS)

Dellith, J; Scheffel, A; Wendt, M

2014-01-01

The KL 2,3 (α) 1,2 -lines of 19 K, the L 3 M 4,5 (α) 1,2 -lines of 48 Cd, and the M 5 N 6,7 (α) 1,2 -lines of 92 U are lines of comparable energy in the region of approximately 3 keV. In none of these cases were we able to resolve the three doublets when recording the spectra in first order Bragg spectrometry using a PET crystal as the dispersing element. For the purpose of enhancing the resolving power of the spectrometer, the three α spectra were recorded in second order reflection, thereby transferring the lines into another spectral region dominated by X-ray quanta of half the energy. In order to achieve high net peak intensities as well as a high peak-to-background ratio and, consequently, a high level of detection capability, the discriminator settings should be optimized quite carefully. In this manner, we were able to resolve the three α doublets and estimate α 2 /α 1 intensity ratios. Inexplicably, current monographs, e.g., by Goldstein et al, do not contain any indications about the rational use of high order spectrometry. Only a few rather old monographs contain some hints in this regard

Scanning electron microscopy-energy dispersive X-ray spectrometer ...

African Journals Online (AJOL)

The distribution of arsenic (As) and cadmium (Cd) in himematsutake was analyzed using scanning electron microscopy-energy dispersive X-ray spectrometer (SEM-EDX). The atomic percentage of the metals was confirmed by inductively coupled plasma-mass spectrometer (ICP-MS). Results show that the accumulation of ...

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

Energy Technology Data Exchange (ETDEWEB)

Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi, E-mail: stx@bnu.edu.cn

2016-04-15

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

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

Energy Technology Data Exchange (ETDEWEB)

Lubeck, J., E-mail: janin.lubeck@ptb.de; Fliegauf, R.; Holfelder, I.; Hönicke, P.; Müller, M.; Pollakowski, B.; Ulm, G.; Weser, J.; Beckhoff, B. [Physikalisch-Technische Bundesanstalt (PTB), Abbestr. 2-12, 10587 Berlin (Germany); Bogovac, M.; Kaiser, R. B.; Karydas, A. G.; Leani, J. J.; Migliori, A.; Sghaier, H. [Nuclear Science and Instrumentation Laboratory, IAEA Laboratories, A-2444, Seibersdorf (Austria); Boyer, B.; Lépy, M. C.; Ménesguen, Y. [CEA, LIST, Laboratoire National Henri Becquerel, Bât. 602 PC 111, CEA-Saclay 91191 Gif-sur-Yvette c. (France); Detlefs, B. [CEA-LETI, Minatec Campus, 17 rue des Martyrs, 38054 Grenoble (France); Eichert, D. [Elettra - Sincrotrone Trieste (EST) S.C.p.A., 34149 Basovizza, Trieste (Italy); and others

2016-07-27

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

Asian conference on x-rays and related techniques in research and industry. Proceedings

International Nuclear Information System (INIS)

1996-01-01

This proceedings compile the paper presented at the conference. The papers for presentation are from wide spectrum stressing the interdisciplinary nature of the conference i.e. x-ray fluorescence spectrometry (XRF), x-ray diffraction (XRD), TEM, scanning electron microscope (SEM), energy dispersive x-ray (EDX), auger electron microscopy, electron back scatter diffraction (EBSD)

Energy Dispersive X-Ray Fluorescence Spectrometric Study of ...

African Journals Online (AJOL)

MBI

2017-06-11

Jun 11, 2017 ... Compositional Differences in Trace Elements in Dried Moringa oleifera ... Ti, Cu, Mo, Fe, Zn, Ni, Re, Eu and Pb using Energy Dispersive X-ray fluorescence ... Africa, Southeast Asia (Valdez-Solana et al., 2015). ... vegetable in many countries, including Nigeria .... of other elements in environmental samples.

Diffraction anomalous fine structure using X-ray anomalous dispersion

International Nuclear Information System (INIS)

Soejima, Yuji; Kuwajima, Shuichiro

1998-01-01

A use of X-ray anomalous dispersion effects for structure investigation has recently been developed by using synchrotron radiation. One of the interesting method is the observation of anomalous fine structure which arise on diffraction intensity in energy region of incident X-ray at and higher than absorption edge. The phenomenon is so called Diffraction Anomalous Fine Structure (DAFS). DAFS originates in the same physical process an that of EXAFS: namely photoelectric effect at the corresponding atom and the interaction of photoelectron waves between the atom and neighboring atoms. In contrast with EXAFS, the method is available for only the crystalline materials, but shows effective advantages of the structure investigations by a use of diffraction: one is the site selectivity and the other is space selectivity. In the present study, demonstrations of a use of X-ray anomalous dispersion effect for the superstructure determination will be given for the case of PbZrO 3 , then recent trial investigations of DAFS in particular on the superlattice reflections will be introduced. In addition, we discuss about Forbidden Reflection near Edge Diffraction (FRED) which is more recently investigated as a new method of the structure analysis. (author)

Determination of zinc in ammoniacal ore leaching solutions by X-ray fluorescence spectrometry using a radioactive source

International Nuclear Information System (INIS)

Cornejo, N.; Afailal, A.; Garcia, F.; Palacios, M.

1994-01-01

A method was developed for the fast determination of zinc in leaching solutions by radioisotope energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The measured intensities were used to develop regression models for estimating the zinc concentration. The primary radiation was provided by the 244 Cm radioisotope. Several experimental parameters including the saturation thickness and detection limit were determined. The advantages of the utilization of conditioning agents with elements of low atomic number such as nitric acid were established. (orig.)

X-ray fluorescence spectrometry applied to soil analysis

International Nuclear Information System (INIS)

Salvador, Vera Lucia Ribeiro; Sato, Ivone Mulako; Scapin Junior, Wilson Santo; Scapin, Marcos Antonio; Imakima, Kengo

1997-01-01

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

Energy-dispersive X-ray microanalysis of elements' content and ...

African Journals Online (AJOL)

This study was designed to investigate elements' content and anti-microbial effects of two Malaysian plants, Pereskia bleo and Goniothalamus umbrosus. Elements' analysis was carried out using Energy Dispersive X-ray Microanalysis combined with Variable Pressure Scanning Electron Microscope (EDX, VPSEM).

Heavy metal determination by X-rays spectrometry in superficial sediments at Havana Bay

International Nuclear Information System (INIS)

Gelen, Alina; Izquierdo, Walter; Lopez, Neivy; Corrales, Yasser; Casanova, Amaya O.; Diaz, Oscar; Manso, Maria V.; D'Alessandro, Katia; Reyes, Enma; Toledo, Carlos; Beltran, Jesus; Perez, Marlen; Ramirez, Marta; Soto, Jesus

2007-01-01

Havana Bay is a typical bag-type located in the Western-North Coast of the Republic of Cuba. Since 1980 it has been the object of a study for sea bottom rehabilitation and improvement of quality of the waters, where the final objective will be the recovery of the coastal and marine ecosystem. Thirteen surface samples of the Havana Bay (Cuba) were collected and analysed by X-Rays spectrometry. Some majority elements (Si, Ca, K, Na, S, Cl, Al, Fe, Mg, C and O) were measured by scanning electron microscopy (SEM) coupled with microanalysis to perform geomorphologic analysis. Nine elements (Ca, Fe, Ti, Mn, Cu, Zn, Sr, Zr and Pb) have been measured using an Energy Dispersive X-Ray Fluorescence (EDXRF) with a Si(Li) detector. Multivariate statistical was used for the analysis. The concentration levels showed this bay as the most polluted in Cuba. The highest contents of Cu, Zn and Pb were obtained in Atares and Marimelena Cove; these elements are indicators of urban as well as industrial pollution. (author)

Heavy metal determination by X-rays spectrometry in superficial sediments at Havana Bay

Energy Technology Data Exchange (ETDEWEB)

Gelen, Alina; Izquierdo, Walter; Lopez, Neivy; Corrales, Yasser; Casanova, Amaya O.; Diaz, Oscar; Manso, Maria V.; D' Alessandro, Katia [Institute for Applied Sciences and Technology, Havana (Cuba)], E-mail: alina@instec.cu; Reyes, Enma; Toledo, Carlos [Central Laboratory Criminology, Havana (Cuba); Beltran, Jesus; Perez, Marlen; Ramirez, Marta [Engineering Centre for Environmental Management of Bays and Coasts, Havana (Cuba)], E-mail: beltran@cimab.transnet.cu; Soto, Jesus [Universidad de Cantabria, Santander (Spain)], E-mail: sotoj@unican.es

2007-07-01

Havana Bay is a typical bag-type located in the Western-North Coast of the Republic of Cuba. Since 1980 it has been the object of a study for sea bottom rehabilitation and improvement of quality of the waters, where the final objective will be the recovery of the coastal and marine ecosystem. Thirteen surface samples of the Havana Bay (Cuba) were collected and analysed by X-Rays spectrometry. Some majority elements (Si, Ca, K, Na, S, Cl, Al, Fe, Mg, C and O) were measured by scanning electron microscopy (SEM) coupled with microanalysis to perform geomorphologic analysis. Nine elements (Ca, Fe, Ti, Mn, Cu, Zn, Sr, Zr and Pb) have been measured using an Energy Dispersive X-Ray Fluorescence (EDXRF) with a Si(Li) detector. Multivariate statistical was used for the analysis. The concentration levels showed this bay as the most polluted in Cuba. The highest contents of Cu, Zn and Pb were obtained in Atares and Marimelena Cove; these elements are indicators of urban as well as industrial pollution. (author)

Soft X ray spectrometry at high count rates

International Nuclear Information System (INIS)

Blanc, P.; Brouquet, P.; Uhre, N.

1978-06-01

Two modifications of the classical method of X-ray spectrometry by a semi-conductor diode permit a count rate of 10 5 c/s with an energy resolution of 350 eV. With a specially constructed pulse height analyzer, this detector can measure four spectra of 5 ms each, in the range of 1-30 keV, during a plasma shot

Application of neutron activation techniques and x-ray energy dispersion spectrometry, in analysis of metallic traces adsorbed by chelex-100 resin; Ativacao das tecnicas de ativacao neutronica e espectrometria por dispersao de onda e de energia de raios X, na analise de tracos metalicos adsorvidos pela resina chelex-100

Energy Technology Data Exchange (ETDEWEB)

Fernandes, Jair C.; Amaral, Angela M.; Magalhaes, Jesus C.; Pereira, Jose S.J.; Silva, Juliana B. da; Auler, Lucia M.L.A. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN), Belo Horizonte, MG (Brazil)]. E-mail: jcf@urano.cdtn.br

2000-07-01

In this work, the authors have investigated optimal conditions of adsorption for several ion metallic groups (cations of heavy metals and transition metals, oxyanions metallics and metalloids and cations of rare earths), as traces (ppb), withdrawn and in mixture of groups, by chelex-100 resin. The experiments have been developed by bath techniques in ammonium acetate tamponade solution 40 mM pH 5,52 content 0,5 g of chelex-100 resin. After magnetic agitation for two hours, resins were dried and submitted to X-ray energy dispersion spectrometry, x-ray fluorescence spectrometry and neutron activation analysis. The results have demonstrated that chelex-100 resin adsorb quantitatively transition element groups and rare earth groups in two cases (withdrawn and simultaneously adsorption)

Analysis of kiwi fruit (Accented deliciosa) by energy dispersive X-ray fluorescence spectra

International Nuclear Information System (INIS)

Oliveira, Ana Claudia S.; Oliveira, Marcia L. de; Silva, Lucia C.A.S.; Arthur, Valter; Almeida, Eduardo

2011-01-01

The search for a healthy life has led consumers to eat fruits and vegetables in place of manufactured products, however, the demand for minimally processed products has evolved rapidly. The kiwi has at least eight nutrients beneficial to health: calcium, magnesium, manganese, phosphorus, iron, potassium, sodium and has also high vitamin C, which has wide acceptance in consumer markets. Energy dispersive spectroscopy X-ray (EDX) is the analytical technique used for elemental analysis or chemical characterization of a sample. It is a variant of fluorescence spectroscopy X-ray based on the sample through an investigation of interactions between electromagnetic radiation and matter, analyzing X-rays emitted by matter in response to being struck by charged particles. The aim of this study were to determine potassium, calcium, iron and bromine (K, Ca, Fe and Br, respectively) present in kiwifruit using the technique of fluorescence X-ray energy dispersive (EDXRF). Kiwifruit were peeled, washed and cut into slices and freeze-dried. After drying the sample was held digestion and subsequent reading of the same equipment in the X-ray fluorescence energy dispersive (EDXRF). The results indicated that the contents of potassium, calcium, iron and bromine are present in kiwifruit as expected when compared to Brazilian Table of Food Composition. (author)

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

DEFF Research Database (Denmark)

Kunzendorf, Helmar; Wollenberg, H.A.

1970-01-01

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

X-Ray Fluorescence Spectrometry. II. Determination of Uranium in ores

International Nuclear Information System (INIS)

Bermudez Polonio, J.; Crus Castillo, F. de la; Fernandez Cellini, R.

1961-01-01

A method of analysis of uranium in ores by X-ray spectrometry was developed, using the internal standard technique. Strontium was found to be the most suitable internal standard for general use. A Norelco Philips X-ray fluorescent spectrometer was used in this work, equipped with a lithium fluoride crystal acting as a diffraction grating analyzer. The intensity of the uranium-L α 1 spectral line is calculated and related to corresponding strontium-K α spectral line, both detected with a Scintillation Counter. (Author) 31 refs

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

Indian Academy of Sciences (India)

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-04-21

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

Quantitative schemes in energy dispersive X-ray fluorescence implemented in AXIL

International Nuclear Information System (INIS)

Tchantchane, A.; Benamar, M.A.; Tobbeche, S.

1995-01-01

E.D.X.R.F (Energy Dispersive X-ray Fluorescence) has long been used for quantitative analysis of many types of samples including environment samples. the software package AXIL (Analysis of x-ray spectra by iterative least quares) is extensively used for the spectra analysis and the quantification of x-ray spectra. It includes several methods of quantitative schemes for evaluating element concentrations. We present the general theory behind each scheme implemented into the software package. The spectra of the performance of each of these quantitative schemes. We have also investigated their performance relative to the uncertainties in the experimental parameters and sample description

Energy dispersion X-ray fluorescence techniques in water pollution analysis

International Nuclear Information System (INIS)

Holynska, B.

1980-01-01

Advantages and limitations of energy dispersion X-ray fluorescence methods for analysis of pollutants in water are discussed. The necessary equipment for X-ray measurement of insoluble and dissolved trace metals in water is described. Different techniques of enrichment of trace metals are presented: ion exchange on selective Chelex-100 exchanger, precipitation with chelating agents DDTC and APDC, and adsorption on activated carbon. Some results obtained using different preconcentration methods for trace metals determination in different waters are presented. (author)

Inference of the phase-to-mechanical property link via coupled X-ray spectrometry and indentation analysis: Application to cement-based materials

Energy Technology Data Exchange (ETDEWEB)

Krakowiak, Konrad J.; Wilson, William [Department of Civil and Environmental Engineering, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, MA 02139-4307 (United States); James, Simon [Schlumberger Riboud Product Center, 1 Rue Henri Becquerel, Clamart 92140 (France); Musso, Simone [Schlumberger-Doll Research Center, 1 Hampshire St., Cambridge, MA 02139-1578 (United States); Ulm, Franz-Josef, E-mail: ulm@mit.edu [Department of Civil and Environmental Engineering, Massachusetts Institute of Technology, 77 Massachusetts Avenue, Cambridge, MA 02139-4307 (United States)

2015-01-15

A novel approach for the chemo-mechanical characterization of cement-based materials is presented, which combines the classical grid indentation technique with elemental mapping by scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDS). It is illustrated through application to an oil-well cement system with siliceous filler. The characteristic X-rays of major elements (silicon, calcium and aluminum) are measured over the indentation region and mapped back on the indentation points. Measured intensities together with indentation hardness and modulus are considered in a clustering analysis within the framework of Finite Mixture Models with Gaussian component density function. The method is able to successfully isolate the calcium-silica-hydrate gel at the indentation scale from its mixtures with other products of cement hydration and anhydrous phases; thus providing a convenient means to link mechanical response to the calcium-to-silicon ratio quantified independently via X-ray wavelength dispersive spectroscopy. A discussion of uncertainty quantification of the estimated chemo-mechanical properties and phase volume fractions, as well as the effect of chemical observables on phase assessment is also included.

Automatic sample changer system for a chain of X-Ray Spectrometry

International Nuclear Information System (INIS)

Kall, B.

2004-01-01

Nowadays, the science evolves and the used techniques become more pointed. At the same time, instruments are more powerful. This rule also applies in the domain of the nuclear science. The object of these works goes in this sense and touch the branch of the X-Ray spectrometry and that brings back himself to the conception and the realization of an automatic sample changer system for the chain of X-Ray Spectrometry. Baptized KEN-001 , it is an instrument of sample changer ordered from certain distance. Indeed, the sample carriers are placed of advance in compartments on its tray and by a control, KEN-001 put one by one those reflectors in the carries reflective for analysis. Once the analysis is finished, the system is in charge of taking and replacing the reflector in its compartment of origin. Of this way, one wins in time and therefore in number of analysis to do in an interval of time given. This instrument of precision contributes to the improvement of the analysis and the evolution of the technique of the X-Ray fluorescence [fr

High Resolution, Non-Dispersive X-Ray Calorimeter Spectrometers on EBITs and Orbiting Observatories

Science.gov (United States)

Porter, Frederick S.

2010-01-01

X-ray spectroscopy is the primary tool for performing atomic physics with Electron beam ion trap (EBITs). X-ray instruments have generally fallen into two general categories, 1) dispersive instruments with very high spectral resolving powers but limited spectral range, limited count rates, and require an entrance slit, generally, for EBITs, defined by the electron beam itself, and 2) non-dispersive solid-state detectors with much lower spectral resolving powers but that have a broad dynamic range, high count rate ability and do not require a slit. Both of these approaches have compromises that limit the type and efficiency of measurements that can be performed. In 1984 NASA initiated a program to produce a non-dispersive instrument with high spectral resolving power for x-ray astrophysics based on the cryogenic x-ray calorimeter. This program produced the XRS non-dispersive spectrometers on the Astro-E, Astro-E2 (Suzaku) orbiting observatories, the SXS instrument on the Astro-H observatory, and the planned XMS instrument on the International X-ray Observatory. Complimenting these spaceflight programs, a permanent high-resolution x-ray calorimeter spectrometer, the XRS/EBIT, was installed on the LLNL EBIT in 2000. This unique instrument was upgraded to a spectral resolving power of 1000 at 6 keV in 2003 and replaced by a nearly autonomous production-class spectrometer, the EBIT Calorimeter Spectrometer (ECS), in 2007. The ECS spectrometer has a simultaneous bandpass from 0.07 to over 100 keV with a spectral resolving power of 1300 at 6 keV with unit quantum efficiency, and 1900 at 60 keV with a quantum efficiency of 30%. X-ray calorimeters are event based, single photon spectrometers with event time tagging to better than 10 us. We are currently developing a follow-on instrument based on a newer generation of x-ray calorimeters with a spectral resolving power of 3000 at 6 keV, and improved timing and measurement cadence. The unique capabilities of the x-ray

Material specific X-ray imaging using an energy-dispersive pixel detector

Energy Technology Data Exchange (ETDEWEB)

Egan, Christopher K., E-mail: christopher.egan@manchester.ac.uk [School of Materials, University of Manchester, Manchester M13 9PL (United Kingdom); Wilson, Matthew D.; Veale, Matthew C.; Seller, Paul [STFC Rutherford Appleton Laboratory, Harwell, Didcot, Oxfordshire OX11 0QX (United Kingdom); Jacques, Simon D.M.; Cernik, Robert J. [School of Materials, University of Manchester, Manchester M13 9PL (United Kingdom)

2014-04-01

By imaging the X-ray spectral properties or ‘colours’ we have shown how material specific imaging can be performed. Using a pixelated energy-dispersive X-ray detector we record the absorbed and emitted hard X-radiation and measure the energy (colour) and intensity of the photons. Using this technology, we are not only able to obtain attenuation contrast but also to image chemical (elemental) variations inside objects, potentially opening up a very wide range of applications from materials science to medical diagnostics.

A low cost multi-purpose experimental arrangement for variants in energy dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Nascimento Filho, V.F.; Silva, R.M.C.; Moraes, L.M.B.; Parreira, P.S.; Appoloni, R.C.; Silva, R.M.C.

2005-01-01

Based in an X-ray tower with four exits (two line and two point beams) experimental conditions were arranged to carry out variants in energy dispersive X-ray fluorescence analysis: (1) the conventional one (EDXRF), with excitation/detection of thin and thick samples, under vacuum and air atmosphere, (2) the X-ray energy dispersive micro- fluorescence analysis(μ-EDXRF), with 2D mapping, using a quartz capillar, (3) the total reflection X-ray fluorescence (TXRF), under He and air atmosphere, and (4) secondary target/polarized X-ray fluorescence (P-EDXRF). It was possible to use a Cu, Mo or W target on the X-ray tube, with or without filter (V, Fe, Ni and Zr), and Si(Li) or Si-PIN semicondutor detectors coupled to a multichannel analyzer. In addition, it was possible to use the point beam to carry out experiments on (5) X-ray radiography and (6) X-ray absorption, and the line beam on (7) X-ray diffractometry studies.

X-Ray Spectrometry for Preventive Conservation Research

International Nuclear Information System (INIS)

Grieken, V. R.

2008-01-01

Preventive conservation studies the influence of environmental conditions on the durability of works of art. X-ray spectrometry (XRS), in its many forms, is one of the main physical analysis techniques used in the context of cultural heritage in view of its non-destructive nature; it is also highly indicated for studying the composition of e.g. harmful atmospheric particles in e.g. museums. A short literature overview will be to illustrate the important role of XRS in conservation. Then some of our own applications of XRS (especially automated electron probe X-ray microanalysis for individual atmospheric particles) will be shown. These include studies in the Wawel Castle in Cracow, Poland (where outdoor soot nanoparticles and deicing salts brought in by visitors were most threatening for the wall tapestry collections) and the Metropolitan Museum in New York, USA (where sodium nitrate particles from the reaction of sea spray with car exhaust gases were predominant in some rooms)

Spectrum unfolding in X-ray spectrometry using the maximum entropy method

International Nuclear Information System (INIS)

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

2014-01-01

The solution of the unfolding problem is an ever-present issue in X-ray spectrometry. The maximum entropy technique solves this problem by taking advantage of some known a priori physical information and by ensuring an outcome with only positive values. This method is implemented in MAXED (MAXimum Entropy Deconvolution), a software code contained in the package UMG (Unfolding with MAXED and GRAVEL) developed at PTB and distributed by NEA Data Bank. This package contains also the code GRAVEL (used to estimate the precision of the solution). This article introduces the new code UMESTRAT (Unfolding Maximum Entropy STRATegy) which applies a semi-automatic strategy to solve the unfolding problem by using a suitable combination of MAXED and GRAVEL for applications in X-ray spectrometry. Some examples of the use of UMESTRAT are shown, demonstrating its capability to remove detector artifacts from the measured spectrum consistently with the model used for the detector response function (DRF). - Highlights: ► A new strategy to solve the unfolding problem in X-ray spectrometry is presented. ► The presented strategy uses a suitable combination of the codes MAXED and GRAVEL. ► The applied strategy provides additional information on the Detector Response Function. ► The code UMESTRAT is developed to apply this new strategy in a semi-automatic mode

Using angular dispersion and anomalous transmission to shape ultramonochromatic x rays

Energy Technology Data Exchange (ETDEWEB)

Shvyd' ko, Yuri; Stoupin, Stanislav; Shu, Deming; Khachatryan, Ruben [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

2011-11-15

Optical spectrometers, instruments that work with highly monochromatic light, are commonly rated by the spectral bandwidth, which defines the ability to resolve closely spaced spectral components. Another equally important feature is the spectral contrast, the ability to detect faint objects among these components. Here we demonstrate that a combined effect of angular dispersion (AD) and anomalous transmission (AT) of x rays in Bragg reflection from asymmetrically cut crystals can shape spectral distributions of x rays to profiles with high contrast and small bandwidths. The AD and AT x-ray optics is implemented as a five-reflection, three-crystal arrangement featuring a combination of the above-mentioned attributes so desirable for x-ray monochromators and analyzers: a spectral contrast of {approx_equal} 500, a bandwidth of {approx_equal} 0.46 meV, and a remarkably large angular acceptance of {approx_equal} 107 {mu}rad with 9.1 keV x rays. The new optics can become a foundation for the next-generation inelastic x-ray scattering spectrometers for studies of atomic dynamics.

Soft X-ray-induced decomposition of amino acids: An XPS, mass spectrometry, and NEXAFS study

International Nuclear Information System (INIS)

Zubavichus, Yan; Fuchs, Oliver; Weinhardt, Lothar; Heske, Clemens; Umbach, Eberhard; Denlinger, Jonathan D.; Grunze, Michael

2003-01-01

Decomposition of five amino acids, alanine, serine, cysteine, aspartic acid, and asparagine, under irradiation with soft X-rays (magnesium Ka X-ray source) in ultra-high vacuum was studied by means of X-ray photoelectron spectrometry (XPS) and mass spectrometry. A comparative analysis of changes in XPS line shapes, stoichiometry and residual gas composition indicates that the molecules decompose by several pathways. Dehydration, decarboxylation, decarbonylation,deamination and desulfurization of pristine molecules accompanied by desorption of H2, H2O, CO2, CO, NH3and H2S are observed with rates depending on the specific amino acid. NEXAFS spectra of cysteine at the carbon, oxygen and nitrogen K-shell and sulfur L2,3 edges complement the XPS and mass spectrometry data and show that the exposure of the sample to an intense soft X-ray synchrotron beam results in the formation of C-C and C-N double and triple bonds. Qualitatively, the amino acids studied can be arranged in the following ascending order of radiation stability:serine< alanine< aspartic acid< cysteine< asparagine

Cu,Cr and As determination in preserved woods (Eucalyptus ssp.) by X-ray fluorescence spectrometries; Determinacao de cobre, cromo e arsenio em madeira preservada (Eucalyptus sp.) pelas espectrometrias de fluorescencia de raios X

Energy Technology Data Exchange (ETDEWEB)

Pereira Junior, Sergio Matias

2014-07-01

Brazil produces around 2.2 millions of cubic meters of treated wood to meet the annual demand of railway, electric, rural and construction sectors. The most used wood species are eucalyptus (Eucalyptus ssp.) and pine (Pinus ssp.).The treated woods used for poles, sleepers, fence posts and plywoods should be according to Brazilian norms requirements. The most usual wood preservative products used in Brazil are CCA (chromated copper arsenate) and CCB (copper chromium and boron salt). The analytical methods, such as flame atomic absorption spectrometry (FAAS), plasma inductively coupled optical emission spectrometry (ICPOES) and X-ray fluorescence spectrometry (XRFS) have been used for the analytical control of those treatment processes. In this work, the eucalyptus trees (Eucalyptus ssp) samples was obtained from Minas Gerais State, Brazil, cut plantation areas. Under pressure, eucalyptus wood samples were submitted to different concentration of CCA solution reaching 3.9, 6.7, 9.1, 12.4 and 14.0 kg of CCA by m-³ sapwood retentions. Samples in cylinders and sawdust forms were obtained from treated wood samples. Copper, chromium and arsenic determination was performed using the energy dispersive X-ray fluorescence spectrometry (EDXRFS), portable X-ray fluorescence spectrometry (PXRFS), flame atomic absorption spectrometry (FAAS) and instrumental neutron activation analysis. In this work, the method of analysis, sensitivity, precision and accuracy performances of the related techniques were outlined. (author)

Photon Counting Energy Dispersive Detector Arrays for X-ray Imaging.

Science.gov (United States)

Iwanczyk, Jan S; Nygård, Einar; Meirav, Oded; Arenson, Jerry; Barber, William C; Hartsough, Neal E; Malakhov, Nail; Wessel, Jan C

2009-01-01

The development of an innovative detector technology for photon-counting in X-ray imaging is reported. This new generation of detectors, based on pixellated cadmium telluride (CdTe) and cadmium zinc telluride (CZT) detector arrays electrically connected to application specific integrated circuits (ASICs) for readout, will produce fast and highly efficient photon-counting and energy-dispersive X-ray imaging. There are a number of applications that can greatly benefit from these novel imagers including mammography, planar radiography, and computed tomography (CT). Systems based on this new detector technology can provide compositional analysis of tissue through spectroscopic X-ray imaging, significantly improve overall image quality, and may significantly reduce X-ray dose to the patient. A very high X-ray flux is utilized in many of these applications. For example, CT scanners can produce ~100 Mphotons/mm(2)/s in the unattenuated beam. High flux is required in order to collect sufficient photon statistics in the measurement of the transmitted flux (attenuated beam) during the very short time frame of a CT scan. This high count rate combined with a need for high detection efficiency requires the development of detector structures that can provide a response signal much faster than the transit time of carriers over the whole detector thickness. We have developed CdTe and CZT detector array structures which are 3 mm thick with 16×16 pixels and a 1 mm pixel pitch. These structures, in the two different implementations presented here, utilize either a small pixel effect or a drift phenomenon. An energy resolution of 4.75% at 122 keV has been obtained with a 30 ns peaking time using discrete electronics and a (57)Co source. An output rate of 6×10(6) counts per second per individual pixel has been obtained with our ASIC readout electronics and a clinical CT X-ray tube. Additionally, the first clinical CT images, taken with several of our prototype photon-counting and

Design of a tritium gas cell for beta-ray induced X-ray spectrometry using Monte Carlo simulation

Energy Technology Data Exchange (ETDEWEB)

Hara, Masanori, E-mail: masahara@ctg.u-toyama.ac.jp [Hydrogen Isotope Research Center, Organization for Promotion of Research, University of Toyama, 3190 Gofuku, Toyama City, Toyama 930-8555 (Japan); Abe, Shinsuke; Matsuyama, Masao [Hydrogen Isotope Research Center, Organization for Promotion of Research, University of Toyama, 3190 Gofuku, Toyama City, Toyama 930-8555 (Japan); Aso, Tsukasa [Electronics and Computer Engineering, National Institute of Technology, Toyama College, 1-2 Ebie-neriya, Imizu City, Toyama 933-0293 (Japan); Tatenuma, Katsuyoshi; Kawakami, Tomohiko; Ito, Takeshi [KAKEN Company Limited, 1044 Horimachi, Mito City, Ibaraki 310-0903 (Japan)

2017-06-15

Highlights: • Beta-ray induced X-ray spectrometry (BIXS) is a method for tritium gas analysis. • Gas cell for BIXS was designed by Monte Carlo simulations. • The optimum thickness of the gold layer on a beryllium window was around 150 nm. • This simulation model considered the self-absorption with increasing the cell length. - Abstract: One of the methods used for tritium gas analysis is beta-ray induced X-ray spectrometry (BIXS). Gas cell design is important in this method. The structure of the gas cell for BIXS was optimized by Monte Carlo simulation of beta-ray induced X-ray spectra in various window geometries using the Geant4 tool kit (version 10.01.p02). The simulated spectrum from tritium decay fitted the observed one, and the simulation model was used to obtain the cell parameters for BIXS. The optimum thickness of the gold layer on a beryllium window was around 150 nm. This simulation model also considered the relationship between self-absorption by hydrogen gas and the cell length. Self-absorption increased with increasing cell length and the relationship between the sample pressure and cell length was formulated.

A Soft X-ray Spectrometer using a Highly Dispersive Multilayer Grating

International Nuclear Information System (INIS)

Warwick, Tony; Padmore, Howard; Voronov, Dmitriy; Yashchuk, Valeriy

2010-01-01

There is a need for higher resolution spectrometers as a tool for inelastic x-ray scattering. Currently, resolving power around R = 10,000 is advertised. Measured RIXS spectra are often limited by this instrumental resolution and higher resolution spectrometers using conventional gratings would be prohibitively large. We are engaged in a development program to build blazed multilayer grating structures for diffracting soft x-rays in high order. This leads to spectrometers with dispersion much higher than is possible using metal coated-gratings. The higher dispersion then provides higher resolution and the multilayer gratings are capable of operating away from grazing incidence as required. A spectrometer design is presented with a total length 3.8 m and capable of 10 5 resolving power.

A Soft X-ray Spectrometer using a Highly Dispersive Multilayer Grating

International Nuclear Information System (INIS)

Warwick, Tony; Padmore, Howard; Voronov, Dmitriy; Yashchuk, Valeriy

2010-01-01

There is a need for higher resolution spectrometers as a tool for inelastic x-ray scattering. Currently, resolving power around R = 10,000 is advertised. Measured RIXS spectra are often limited by this instrumental resolution and higher resolution spectrometers using conventional gratings would be prohibitively large. We are engaged in a development program to build blazed multilayer grating structures for diffracting soft x-rays in high order. This leads to spectrometers with dispersion much higher than is possible using metal coated-gratings. The higher dispersion then provides higher resolution and the multilayer gratings are capable of operating away from grazing incidence as required. A spectrometer design is presented with a total length 3.8m and capable of 10 5 resolving power.

Scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and aerosol time-of-flight mass spectrometry (ATOFMS) single particle analysis of metallurgy plant emissions

International Nuclear Information System (INIS)

Arndt, J.; Deboudt, K.; Anderson, A.; Blondel, A.; Eliet, S.; Flament, P.; Fourmentin, M.; Healy, R.M.; Savary, V.; Setyan, A.; Wenger, J.C.

2016-01-01

The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe–Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy–energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site. - Highlights: • Similar composition for emitted particles as those collected on the chimney filters. • Emitted particles dominated by Ca-, Mn and/or Al-containing particles. • Identification of specific particle types emitted by the different process units. - The particles emitted by metallurgy activities are fully described by ATOFMS and SEM-EDX, enabling the identification of specific particle types from the different units of the process.

Gaseous detectors for energy dispersive X-ray fluorescence analysis

Science.gov (United States)

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.

Measurement of grain size of polycrystalline materials with confocal energy dispersive micro-X-ray diffraction technology based on polycapillary X-ray optics

Energy Technology Data Exchange (ETDEWEB)

Sun, Weiyuan; Liu, Zhiguo [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Sun, Tianxi, E-mail: stx@bnu.edu.cn [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Peng, Song [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Ma, Yongzhong [Center for Disease Control and Prevention of Beijing, Beijing 100013 (China); Li, Fangzuo; Sun, Xuepeng; Ding, Xunliang [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China)

2014-11-11

The confocal energy dispersive micro-X-ray diffraction (EDMXRD) based on polycapillary X-ray optics was used to determine the grain size of polycrystalline materials. The grain size of a metallographic specimen of nickel base alloy was measured by using the confocal EDMXRD. The experimental results demonstrated that the confocal EDMXRD had potential applications in measuring large grain size.

Dispersive x-ray synchrotron studies of Pt-C multilayers

International Nuclear Information System (INIS)

Smither, R.K.; Rodricks, B.; Lamelas, F.; Medjahed, D.; Dos Passos, W.; Clarke, R.; Ziegler, E.; Fontaine, A.

1989-02-01

We demonstrate the simultaneous acquisition of high-resolution x-ray absorption spectra and scattering data, using a combination of energy-dispersive optics and a two-dimensional CCD detector. Results are presented on the optical constants of Pt and on the reflectivity of a platinum-carbon multilayer at the L/sub III/ absorption edge of Pt. 12 refs., 5 figs

Single atom identification by energy dispersive x-ray spectroscopy

International Nuclear Information System (INIS)

Lovejoy, T. C.; Dellby, N.; Krivanek, O. L.; Ramasse, Q. M.; Falke, M.; Kaeppel, A.; Terborg, R.; Zan, R.

2012-01-01

Using aberration-corrected scanning transmission electron microscope and energy dispersive x-ray spectroscopy, single, isolated impurity atoms of silicon and platinum in monolayer and multilayer graphene are identified. Simultaneously acquired electron energy loss spectra confirm the elemental identification. Contamination difficulties are overcome by employing near-UHV sample conditions. Signal intensities agree within a factor of two with standardless estimates.

Energy-dispersive X-ray fluorescence – A tool for interdisciplinary ...

Indian Academy of Sciences (India)

Keywords. Energy-dispersive X-ray fluorescence; trace elements; oral cancer; biomonitoring; air pollution. Abstract. Trace elements have been at the focus of attention for decades with considerable emphasis on their role in biology and biomedical sciences, environmental sciences, geology, archaeology and material ...

Quantitative analysis of phosphosilicate glass films on silicon wafers for calibration of x-ray fluorescence spectrometry standards

International Nuclear Information System (INIS)

Weissman, S.H.

1983-01-01

The phosphorus and silicon contents of phosphosilicate glass films deposited by chemical vapor deposition (CVD) on silicon wafers were determined. These films were prepared for use as x-ray fluorescence (XRF) spectrometry standards. The thin films were removed from the wafer by etching with dilute hydrofluoric acid, and the P and Si concentrations in solution were determined by inductively coupled plasma atomic emission spectroscopy (ICP). The calculated phosphorus concentration ranged from 2.2 to 12 wt %, with an uncertainty of 2.73 to 10.1 relative percent. Variation between the calculated weight loss (summation of P 2 O 5 and SiO 2 amounts as determined by ICP) and the measured weight loss (determined gravimetrically) averaged 4.9%. Results from the ICP method, Fourier transform-infrared spectroscopy (FT-IR), dispersive infrared spectroscopy, electron microprobe, and x-ray fluorescence spectroscopy for the same samples are compared

Physical methods for studying minerals and solid materials: X-ray, electron and neutron diffraction; scanning and transmission electron microscopy; X-ray, electron and ion spectrometry

International Nuclear Information System (INIS)

Eberhart, J.-P.

1976-01-01

The following topics are discussed: theoretical aspects of radiation-matter interactions; production and measurement of radiations (X rays, electrons, neutrons); applications of radiation interactions to the study of crystalline materials. The following techniques are presented: X-ray and neutron diffraction, electron microscopy, electron diffraction, X-ray fluorescence analysis, electron probe microanalysis, surface analysis by electron emission spectrometry (ESCA and Auger electrons), scanning electron microscopy, secondary ion emission analysis [fr

Energy dispersive X-ray fluorescence spectrometry for the direct multi-element analysis of dried blood spots

Science.gov (United States)

Marguí, E.; Queralt, I.; García-Ruiz, E.; García-González, E.; Rello, L.; Resano, M.

2018-01-01

Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients. In this sense, dried blood spots (DBS) are proposed as a non-invasive and even self-administered alternative to sampling whole venous blood. This contribution explores the potential of energy dispersive X-ray fluorescence spectrometry for the simultaneous and direct determination of some major (S, Cl, K, Na), minor (P, Fe) and trace (Ca, Cu, Zn) elements in blood, after its deposition onto clinical filter papers, thus giving rise to DBS. For quantification purposes the best strategy was to use matrix-matched blood samples of known analyte concentrations. The accuracy and precision of the method were evaluated by analysis of a blood reference material (Seronorm™ trace elements whole blood L3). Quantitative results were obtained for the determination of P, S, Cl, K and Fe, and limits of detection for these elements were adequate, taking into account their typical concentrations in real blood samples. Determination of Na, Ca, Cu and Zn was hampered by the occurrence of high sample support (Na, Ca) and instrumental blanks (Cu, Zn). Therefore, the quantitative determination of these elements at the levels expected in blood samples was not feasible. The methodology developed was applied to the analysis of several blood samples and the results obtained were compared with those reported by standard techniques. Overall, the performance of the method developed is promising and it could be used to determine the aforementioned elements in blood samples in a simple, fast and economic way. Furthermore, its non-destructive nature enables further analyses by means of complementary techniques to be carried out.

Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

Indian Academy of Sciences (India)

An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic ...

Combined X-ray CT and mass spectrometry for biomedical imaging applications

Science.gov (United States)

Schioppa, E., Jr.; Ellis, S.; Bruinen, A. L.; Visser, J.; Heeren, R. M. A.; Uher, J.; Koffeman, E.

2014-04-01

Imaging technologies play a key role in many branches of science, especially in biology and medicine. They provide an invaluable insight into both internal structure and processes within a broad range of samples. There are many techniques that allow one to obtain images of an object. Different techniques are based on the analysis of a particular sample property by means of a dedicated imaging system, and as such, each imaging modality provides the researcher with different information. The use of multimodal imaging (imaging with several different techniques) can provide additional and complementary information that is not possible when employing a single imaging technique alone. In this study, we present for the first time a multi-modal imaging technique where X-ray computerized tomography (CT) is combined with mass spectrometry imaging (MSI). While X-ray CT provides 3-dimensional information regarding the internal structure of the sample based on X-ray absorption coefficients, MSI of thin sections acquired from the same sample allows the spatial distribution of many elements/molecules, each distinguished by its unique mass-to-charge ratio (m/z), to be determined within a single measurement and with a spatial resolution as low as 1 μm or even less. The aim of the work is to demonstrate how molecular information from MSI can be spatially correlated with 3D structural information acquired from X-ray CT. In these experiments, frozen samples are imaged in an X-ray CT setup using Medipix based detectors equipped with a CO2 cooled sample holder. Single projections are pre-processed before tomographic reconstruction using a signal-to-thickness calibration. In the second step, the object is sliced into thin sections (circa 20 μm) that are then imaged using both matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) and secondary ion (SIMS) mass spectrometry, where the spatial distribution of specific molecules within the sample is determined. The

Low-energy X-ray and gamma spectrometry using silicon photodiodes

International Nuclear Information System (INIS)

Silva, Iran Jose Oliveira da

2000-08-01

The use of semiconductor detectors for radiation detection has increased in recent years due to advantages they present in comparison to other types of detectors. As the working principle of commercially available photodiodes is similar to the semiconductor detector, this study was carried out to evaluate the use of Si photodiodes for low energy x-ray and gamma spectrometry. The photodiodes investigated were SFH-205, SFH-206, BPW-34 and XRA-50 which have the following characteristics: active area of 0,07 cm 2 and 0,25 cm 2 , thickness of the depletion ranging from 100 to 200 μm and junction capacitance of 72 pF. The photodiode was polarized with a reverse bias and connected to a charge sensitive pre-amplifier, followed by a amplifier and multichannel pulse analyzer. Standard radiation source used in this experiment were 241 Am, 109 Cd, 57 Co and 133 Ba. The X-ray fluorescence of lead and silver were also measured through K- and L-lines. All the measurements were made with the photodiodes at room temperature.The results show that the responses of the photodiodes very linear by the x-ray energy and that the energy resolution in FWHM varied between 1.9 keV and 4.4 keV for peaks corresponding to 11.9 keV to 59 keV. The BPW-34 showed the best energy resolution and the lower dark current. The full-energy peak efficiency was also determined and it was observed that the peak efficiency decreases rapidly above 50 keV. The resolution and efficiency are similar to the values obtained with other semiconductor detectors, evidencing that the photodiodes used in that study can be used as a good performance detector for low energy X-ray and gamma spectrometry. (author)

Analysis of siliceous geologic materials by energy-dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Roca, M.; Bayon, A.

1987-01-01

The determination of the elements Al, Si, K, Ca, Ti, Cr, Mn and Fe in siliceous geologic samples by energy-dispersive X-ray fluorescence is investigated using the most adequate excitation conditions: direct excitation mode (rhodium anode X-ray tube) for the former two elements, and the secondary targets titanium for K and Ca, and germanium for Ti, Cr, Mn and Fe. For the correction of matrix effects the use of ratio methods has been tested. Procedure files have been defined allowing the automatic simultaneous acquisition and processing of spectra. (author)

Application of energy dispersive x-ray techniques for water analysis

International Nuclear Information System (INIS)

Funtua, I. I.

2000-07-01

Energy dispersive x-ray fluorescence (EDXRF) is a class of emission spectroscopic techniques that depends upon the emission of characteristic x-rays following excitation of the atomic electron energy levels by tube or isotopic source x-rays. The technique has found wide range of applications that include determination of chemical elements of water and water pollutants. Three EDXRF systems, the isotopic source, secondary target and total reflection (TXRF) are available at the Centre for Energy research and Training. These systems have been applied for the analysis of sediments, suspensions, ground water, river and rainwater. The isotopic source is based on 55 Fe, 109 Cd and 241 Am excitations while the secondary target and the total reflection are utilizing a Mo x-ray tube. Sample preparation requirements for water analysis range from physical and chemical pre-concentration steps to direct analysis and elements from Al to U can be determined with these systems. The EDXRF techniques, TXRF in particular with its multielement capability, low detection limit and possibility of direct analysis for water have competitive edge over the traditional methods of atomic absorption and flame photometry

Dibenzylammonium and sodium dibenzyldithiocarbamates as precipitants for preconcentration of trace elements in water for analysis by energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Moore, R.V.

1982-01-01

Precipitation with combined dibenzylammonium dibenzyldithiocarbamate and sodium dibenzyldithiocarbamate at pH 5.0 can be used to separate 22 trace elements from water. Membrane filtration of the precipitate yielded a thin sample, suitable for analysis by energy dispersive X-ray fluorescence spectrometry. Alkalis, alkaline earths, lanthanides, and halides were not precipitated, permitting a clean separation of trace elements from the macro constituents of drinking water and drinking water supplies. Methods are given for preparation of reagents of higher purity than previously described

Determination of Cu, Cr, and As in preserved wood (Eucalyptus sp.) using x-ray fluorescent spectrometry techniques

International Nuclear Information System (INIS)

Sergio Matias Pereira Junior; Vera Akiko Maihara; Edson Goncalves Moreira; Vera Lucia Ribeiro Salvador; Ivone Mulako Sato

2016-01-01

Energy dispersive (EDXRF) and Portable (PXRF) X-ray fluorescence techniques are proposed for wood treatment control process and wood waste assortment. In this study, different retentions of chromated copper arsenate preservative were applied to Eucalyptus sp. sapwood samples. Cu, Cr and As were determined by XRF techniques in treated sapwood massive blocks and treated sapwood sawdust samples were analyzed by FAAS spectrometry (Flame Atomic Absorption) and INAA (Instrumental Neutron Activation Analysis). Cu, Cr and As mean values, obtained by FAASS and INAA, showed to be statically equal; however, XRF analysis showed considerable deviations, presenting the absorption and the enhancement effects in analytical lines. (author)

X-ray sky

International Nuclear Information System (INIS)

Gruen, M.; Koubsky, P.

1977-01-01

The history is described of the discoveries of X-ray sources in the sky. The individual X-ray detectors are described in more detail, i.e., gas counters, scintillation detectors, semiconductor detectors, and the principles of X-ray spectrometry and of radiation collimation aimed at increased resolution are discussed. Currently, over 200 celestial X-ray sources are known. Some were identified as nebulae, in some pulsations were found or the source was identified as a binary star. X-ray bursts of novae were also observed. The X-ray radiation is briefly mentioned of spherical star clusters and of extragalactic X-ray sources. (Oy)

Energy dispersive x-ray fluorescence spectrometric determination of phosphorus, calcium, iron, zinc, and strontium in human bones

International Nuclear Information System (INIS)

Ohta, Akishige; Matsubayashi, Takashi; Itoman, Moritoshi

1981-01-01

Phosphorus, calcium, iron, zinc and strontium in a human bone extracted by surgery were determined by energy dispersive X-ray fluorescence spectrometry. The bone was decomposed with nitric acid, then diluted with water. A specific quantity of the solution was naturally dried on polyethylene film, and subjected to X-ray analysis. For determining the calibration curves in a mixture of phosphorus, calcium, iron, zinc and strontium, for the analysis of phosphorus and calcium, germanium was used as the secondary target and aluminum as the filter; and for the analysis of iron, zinc and strontium, molybdenum and molybdenum-aluminum were used, respectively. Consequently, the calibration curves were able to be obtained with high precision in the ranges from 5 to 500 μg of phosphorus, from 1 to 50 μg of calcium and from 0.1 to 1.0 μg of iron, zinc and strontium. In this way, in 1 mg of the human bone by wet weight, phosphorus, calcium, iron, zinc and strontium were able to be determined. (J.P.N.)

Chemical analysis of zinc electroplating solutions by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Jung, Sung-Mo; Cho, Young-Mo; Na, Han-Gil

2007-01-01

A quantitative analysis method used to analyze chlorine, iron and zinc in electroplating solutions, using X-ray spectrometry in atmospheric He mode, is proposed. The present research concerns the replacement of the conventional analyses of electroplating solutions with rapid and reproducible quantification using X-ray fluorescence spectrometer. An in-depth investigation conducted in the present study identifies the species present in the real electroplating solutions. XRD patterns and semi-quantitative results for the electroplating solutions show synthetic standards based on the compositional range of solutions by analyzing the electroplating solutions obtained in real processes. 28 calibration standard solutions are prepared by diluting liquid standard solutions certified by titration and ICP-OES analyses used to construct the XRF calibration curves for Cl, Fe and Zn. The suggested method showed satisfactory precision and accuracy in the analysis of electroplating solutions. The present study provides evidences that the proposed XRF spectrometry could be an alternative analytical method to replace the conventional techniques by comparing the uncertainties estimated for each method. (author)

Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

International Nuclear Information System (INIS)

Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

2013-01-01

Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed. - Author-Highlights: • We measured elemental and chemical composition of raw and activated halloysite mineral samples. • We showed that X-ray techniques allow precise study of changes in the sample composition. • We describe procedure of activation of the samples by etching them in sulfuric acid. • We tested ability of halloysite mineral to absorb lead from contaminated water

X-ray fluorescence spectrometry and related techniques an introduction

CERN Document Server

Margui, Eva

2013-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-11-15

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

Influence of experimental conditions on atom column visibility in energy dispersive X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Dycus, J.H.; Xu, W.; Sang, X. [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way Engineering Building 1, Raleigh, NC 27606 (United States); D' Alfonso, A.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Chen, Z. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); Weyland, M. [Monash Centre for Electron Microscopy, Monash University, Clayton, Victoria 3800 (Australia); Department of Materials Science and Engineering, Monash University, Clayton, Victoria 3800 (Australia); Allen, L.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Findlay, S.D. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); LeBeau, J.M., E-mail: jmlebeau@ncsu.edu [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way Engineering Building 1, Raleigh, NC 27606 (United States)

2016-12-15

Here we report the influence of key experimental parameters on atomically resolved energy dispersive X-ray spectroscopy (EDX). In particular, we examine the role of the probe forming convergence semi-angle, sample thickness, lattice spacing, and dwell/collection time. We show that an optimum specimen-dependent probe forming convergence angle exists to maximize the signal-to-noise ratio of the atomically resolved signal in EDX mapping. Furthermore, we highlight that it can be important to select an appropriate dwell time to efficiently process the X-ray signal. These practical considerations provide insight for experimental parameters in atomic resolution energy dispersive X-ray analysis. - Highlights: • Impacts of microscope operating conditions on EDX signal and atom column contrast are demonstrated. • Influence of sample thickness and lattice spacing is shown. • Conditions for obtaining optimal signal and contrast for different sample types are discussed. • Effects of dwell time during EDX acquisition are discussed.

Application of high resolution x-ray spectrometry preceded by neutron activation for elemental analysis of soil samples

International Nuclear Information System (INIS)

Hernandez Rivero, A.; Capote Rodriguez, G.; Herrera Peraza, E.

1996-01-01

Utilization of High Resolution X-Ray Spectrometry preceded by activation of the samples by irradiation with neutron fluxes (NAA R X) is a relatively modern trend in application of nuclear techniques. This method may complement advantageously the usual Neutron Activation Analysis by means of Gamma Spectrometry (NAA-G) In this work results obtained by the application of NAA-RX for non-destructive analysis of Cuban soil samples are discussed. The samples were irradiated with reactor neutron fluxes and the induced characteristic X-rays were measured by using Si(li)-detector. Concentrations of Fe, Zn and Eu as determined by NAA-RX are compared with both NAA-G and XRF data. For the elaboration of X-ray and Gamma Spectra the computer programs AXIL and ACTAN were used respectively

Elemental analysis of air particulate samples in Jakarta area by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Yumiarti; Yusuf, M.; Mellawati, June; Menry, Yulizon; Surtipanti S

1998-01-01

Determination of elements in air particulate samples collected from Jakarta, especially from industrial area Pulo Gadung, also from residence, office, and recreation sites had been carried out. The samples collected periodically from August through December 1996. The elements were analyzed by X-ray fluorescence spectrometry method. Quantitative and qualitative analyses were done using QXAS AXIL (Quantitative X-ray Analysis System of x-ray Spectra by Iterative Least squares fitting) and QAES (Quantitative Analyses of Environmental Samples) package program. Results of the analyses showed that the content of heavy metal elements in air particulate samples from all areas studied were still below the maximum permissible concentration. (authors)

Application of energy dispersive X-ray spectrometers with semiconductor detectors in radiometric analyses

International Nuclear Information System (INIS)

Jugelt, P.; Schieckel, M.

1983-01-01

Problems and possibilities of applying semiconductor detector spectrometers in radiometric analyses are described. A summary of the state of the art and tendencies of device engineering and spectra evaluation is given. Liquid-nitrogen cooled Li-drifted Si-detectors and high-purity Ge-detectors are compared. Semiconductor detectors working at room temperature are under development. In this connection CdTe and HgI 2 semiconductor detectors are compared. The use of small efficient computers in the spectrometer systems stimulates the development of algorithms for spectra analyses and for determining the concentration. Fields of application of energy dispersive X-ray spectrometers are X-ray diffraction and X-ray macroanalysis in investigating the structure of extensive surface regions

Simultaneous acquisition of X-ray spectra using a multi-wire, position-sensitive gas flow detector

International Nuclear Information System (INIS)

Beaven, Peter A.; Marmotti, Mauro; Kampmann, Reinhard; Knoth, Joachim; Schwenke, Heinrich

2003-01-01

A multi-wire, gas-filled position-sensitive detector has been developed for the simultaneous recording of wavelength-dispersed X-ray signals that enables X-ray fluorescence spectrometry with a limited multi-element capability in the low Z element range. Details of the modular construction of the detector are given. The detector performance was characterized using Al-Kα radiation and a variable slit system. The detector has been applied in a laboratory spectrometer equipped with an electron source and a double multilayer mirror device as the wavelength-dispersing element. Spectra from Al and Si obtained in the simultaneous acquisition mode show good agreement with calculations performed using a ray-tracing model

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-08-01

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

Automatic energy dispersive x-ray fluorescence analysing apparatus

International Nuclear Information System (INIS)

Russ, J.C.; Carey, R.; Chopra, V.K.

1983-01-01

The invention discloses a number of improvements for an energy dispersive X-ray analysis system having computer supervised data collection, display and processing. The systems with which the improved circuitry and methods may be used include a dual interlocking bus structure so that the analyzer and computer functions communicate directly with each other and the user has immediate keyboard control of both. Such a system normally includes a system base control, a control console and a display console. The portions of the system which have been improved include a new type of ratemeter which gives a voltage output proportional to the intensity of the energy window or windows under consideration, an output which is an absolute digital representation of the intensity count rate, circuitry for input multiplexing and multiple output voltage buffering of the ratemeter to accomodate multiple single channel signals, and a new dead time correction to enable meaningful single channel intensity data to be handled by the system. An extension of the ratemeter is also disclosed for use in conjunction with X-ray mapping, enabling enhancements to be made on mapping SCA data

Commercial Applications of X Ray Spectrometric Techniques

Energy Technology Data Exchange (ETDEWEB)

Wegrzynek, D., E-mail: D.Wedgrznek@iaea.org [International Atomic Energy Agency, The IAEA Laboratories, Seibersdorf, Vienna (Austria)

2013-07-15

In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z {>=} 10, with a few instruments capable of detecting also elements with Z {>=} 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg's law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

Evaluation of an automated assay system to measure soil radionuclides by L x-ray and gamma-ray spectrometry

International Nuclear Information System (INIS)

Nyhan, J.W.; Drennon, B.J.; Crowell, J.M.

1982-08-01

An automated radionuclide assay system for conducting soil radioassays using L x-ray and gamma-ray spectrometry was evaluated. Wet chemistry assay procedures were shown to be considerably more time consuming than similar analyses of soil on this radionuclide assay system. The detection limits of 241 Am and plutonium were determined, as well as the reproducibility of radionuclide assay results. The L x-ray spectrometric measurements were compared with radiochemical analyses on several tuff samples. The assay system's intrinsic germanium detector was found to respond linearly to varying low concentrations of 241 Am and plutonium, both of which were easily detected in the presence of elevated concentrations of 137 Cs

X-ray electromagnetic application technology

International Nuclear Information System (INIS)

2011-01-01

The investigating committee aimed at research on electromagnetic fields in functional devices and X-ray fibers for efficient coherent X-ray generation and their material science, high-precision manufacturing, particularly for X-ray electromagnetic application technology from January 2006 to December 2008. In this report, we describe our research results, in particular, on the topics of synchrotron radiation and free-electron laser, Saga Synchrotron Project, X-ray waveguides and waveguide-based lens-less hard-X-ray imaging, X-ray nanofocusing for capillaries and zone plates, dispersion characteristics in photonics crystal consisting of periodic atoms for nanometer waveguides, electromagnetic characteristics of grid structures for scattering fields of nano-meter electromagnetic waves and X-rays, FDTD parallel computing of fundamental scattering and attenuation characteristics of X-ray for medical imaging diagnosis, orthogonal relations of electromagnetic fields including evanescent field in dispersive medium. (author)

New methods of X-ray diffraction spectrometry. II

International Nuclear Information System (INIS)

Soerum, H.; Bremer, J.

1980-01-01

The construction principles for a flexible X-ray spectrometer can be equipped either with a single curved crystal or with two curved crystals are described. A few of the theoretical 4+32 possible working modes are selected for a closer investigation and examples of recorded spectra are given. It is shown in the general single-crystal case that for a wavelength close to a cut-off energy the narrow diffraction cone has an elliptic section, as predicted by the theory. The spectrometer is discussed in terms of intensity, resolution and dispersive power. A comparison with other types of spectrometer is made. (Auth.)

Application of high resolution x-ray spectrometry preceded by neutron activation for elemental analysis of soil samples

International Nuclear Information System (INIS)

Hernandez Rivero, A.; Capote Rodriguez, G.; Padilla Alvarez, R.; Herrera Peraza, E.

1997-01-01

Utilization of High Resolution X-Ray Spectrometry preceded by activation of the samples by irradiation with neutron fluxes (NAA-RX) is a relatively modern trend in application of nuclear techniques. This method may complement advantageously the usual Neutron Activation Analysis by means of Gamma Spectrometry (NAA-G). In this work results obtained by the application of NAA-RX for non-destructive analysis of Cuban soil samples are discussed. The samples were irradiated with reactor neutron fluxes and the induced characteristic X-rays were measured by using Si(Li)-detector. Concentrations of Fe, Zn and Eu as determined by NAA-RX are compared with both NAA-G and XRF data. For the elaboration of X-Ray and Gamma Spectra the computer programs AXIL and ACTAN were used respectively. (author) [es

Applications of the Basic programming language in X-ray spectrometry

International Nuclear Information System (INIS)

Diaz-Guerra, J.P.; Roca, M.

1981-01-01

An assembly of programs written in ''Basic'' language and related with the calculation needs at the X-ray spectrometry laboratory of the Spanish J.E.N. has been developed. The principal problems considered, concerning the X-ray fluorescence technique, are the following: selection of the instrumental parameters; correction of the effects due to the dead time, background and spectral interferences; fitting of polynomial functions, which relate the variables intensity-concentration; application of some empirical-mathematical methods (Lucas-Tooth, Beattie and Brissey and Tertian procedures) to the correction of the inter-element effects; addition method, and statistical treatment of the results (correlation coefficient and ''F'' and ''t'' tests). Likewise, programs for the computation of spacings from powder diffraction patterns (Debye-Scherrer and counter diffractometer procedures) have been written. The proposed programs run following conversational patterns, in which different possibilities and incidences have been foreseen. (author)

Optimization of measure parameters for an X- and gamma-ray spectrometry portable system

International Nuclear Information System (INIS)

Fernandes, Jaquiel S.; Appoloni, Carlos R.

2008-01-01

In order to optimize the use of a system for in situ gamma (γ)- and X-ray spectrometry composed of a 3x3x1 mm 3 Cadmium Telluride (CdTe) detector with respect to the detection of low-activity radioactive sources, a two level factorial planning was accomplished, involving three factors that could modify the system response. This planning was made with a 137 Cs punctual source, analyzing the X-ray energy line of 32 keV from 137m Ba. It was concluded that, for the system optimization, the best configuration for the involved parameters was to work with the detector at temperature of -22 o C, shaping time of 3 μs and rise time discrimination (RTD) with value 3

Energy-dispersive X-ray fluorescence analysis of cerium in ferrosilicon

International Nuclear Information System (INIS)

Marbec, E.R.

1987-01-01

The cerium was determined in ferrosilicon samples by energy-dispersive X-ray fluorescence techniques (XRF) techniques, with a secondary target of gadolinium. The methods employed were: comparison and linear regression with reference materials with cerium concentration between 0.4 and 1.0%. The samples were prepared in the form of pellets and the analytical results are reported as an average of five determinations with a confidence limits at 95% probability. (Author) [es

Challenges for energy dispersive X-ray absorption spectroscopy at the ESRF: microsecond time resolution and Mega-bar pressures

International Nuclear Information System (INIS)

Aquilanti, G.

2002-01-01

This Thesis concerns the development of two different applications of energy-dispersive X-ray absorption spectroscopy at the ESRF: time-resolved studies pushed to the microsecond time resolution and high-pressure studies at the limit of the Mega-bar pressures. The work has been developed in two distinct parts, and the underlying theme has been the exploitation of the capabilities of an X-ray absorption spectrometer in dispersive geometry on a third generation synchrotron source. For time-resolved studies, the study of the triplet excited state following a laser excitation of Pt 2 (P 2 O 5 H 2 ) 4 4- has been chosen to push the technique to the microsecond time resolution. In the high-pressure part, the suitability of the energy dispersive X-ray absorption spectrometer for high-pressure studies using diamond anvils cell is stressed. Some technical developments carried out on beamline ID24 are discussed. Finally, the most extensive scientific part concerns a combined X-ray absorption and diffraction study of InAs under pressure. (author)

X-ray hot plasma diagnostics

International Nuclear Information System (INIS)

Cojocaru, E.

1984-11-01

X-ray plasma emission study is powerful diagnostic tool of hot plasmas. In this review article the main techniques of X-ray plasma emission measurement are shortly presented: X-ray spectrometry using absorbent filters, crystal and grating spectrometers, imaging techniques using pinhole cameras, X-ray microscopes and Fresnel zone plate cameras, X-ray plasma emission calorimetry. Advances in these techniques with examples for different hot plasma devices are also presentes. (author)

Structure investigation of metal ions clustering in dehydrated gel using x-ray anomalous dispersion effect

CERN Document Server

Soejima, Y; Sugiyama, M; Annaka, M; Nakamura, A; Hiramatsu, N; Hara, K

2003-01-01

The structure of copper ion clusters in dehydrated N-isopropylacrylamide/sodium acrylate (NIPA/SA) gel has been studied by means of small angle X-ray scattering (SAXS) method. In order to distinguish the intensity scattered by Cu ions, the X-ray anomalous dispersion effect around the Cu K absorption edge has been coupled with SAXS. It is found that the dispersion effect dependent on the incident X-ray energy is remarkable only at the momentum transfer q = 0.031 A sup - sup 1 , where a SAXS peak is observed. The results indicate that copper ions form clusters in the dehydrated gel, and that the mean size of clusters is the same as that of SA clusters produced by microphase separation. It is therefore naturally presumed that copper ions are adsorbed into the SA molecules. On the basis of the presumption, a mechanism is proposed for microphase-separation and clustering of Cu ions.

Nondestructive analysis of silver in gold foil using synchrotron radiation X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Kasamatsu, Masaaki; Suzuki, Yasuhiro; Suzuki, Shinichi; Nakanishi, Toshio; Shimoda, Osamu; Nishiwaki, Yoshinori; Miyamoto, Naoki

2005-01-01

Small particles of gold foil detached from an indoor decoration might be important evidence to associate a suspect with a crime scene. We have investigated the application of elemental analysis using synchrotron radiation X-ray fluorescence spectrometry to discriminate small particles of gold foil. Eight kinds of gold foil samples collected in Japan were used in the experiments. As a result of synchrotron radiation X-ray fluorescence spectrometry, only two elements, gold and silver, were detected from all gold foil samples. The intensity ratios of AgK α /AuL α showed good correlation with the content ratios of Ag/Au. The variation of intensity ratio within a same sample was sufficiently small compared with those of different samples. Therefore the comparison of this intensity ratio can be an effective method to discriminate small particles originating from different types of gold foil. (author)

Thin coating thickness determination using radioisotope-excited x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Del Castillo, Lorena A.; Calix, Virginia S.

2001-01-01

Three different approaches on thin coating thickness determination using a radioisotope-excited x-ray fluorescence spectrometry were demonstrated and results were compared. A standard of thin layer of gold (Au) on a nickel (Ni) substrate from the US National Bureau of Standards (with a nominal thickness of 0.300505 microns of at least 99.9% Au electrodeposited over 2 nils of Ni) on low carbon steel (1010) was analyzed using a Cd 109-excited XRF system. Au thickness computations were done using the (a) thin standard approach, (b) thick standard approach, and (c) x-ray absorption method (ASTM A754-79 1982). These three methods yielded results within the limit set by the American Society for Testing Materials (ASTM), which is +/-3%. Of the three methods, the thick standard yielded the best result with 0.124% error. (Author)

Analysis of metals in organic compounds by energy dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Anjos, Marcelino J.; Lopes, Ricardo T.; Jesus, Edgar F.O. de

2000-01-01

Using energy dispersive X-ray fluorescence analysis with an X-ray tube filtered with Ti. It was possible to determine the concentration of the elements at ppm level of several elements: K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn As, Rb, Sr, Y, Zr, and Pb in two types of organic compound enough used in the agriculture: organic compound of urban garbage (Fertilurb) and aviary bed (birds manure). The experimental setup is composed of: x-ray tube (Oxford, 30 kV, 50 μA and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray beam is quasi- monochromatic by using Ti filter. The samples were prepared in pellet form with superficial density in the range of 100 mg/cm 2 . The fundamental parameter method was used in order to verify the elemental concentration. The radiation transmission method was going used to the radiation absorption effects correction in the samples. (author)

Determination of some elements along the length of pine needles by means of the scanning energy dispersive x-ray fluorescence (EDXRF) method

International Nuclear Information System (INIS)

Viksna, A.; Katkevics, J.; Nulle, S.

1998-01-01

The scanning energy dispersive X-ray fluorescence (EDXDF) is used to measure the distribution of trace elements along the length of single pine needles. The current set up allows simultaneous determination up to 15 trace elements. The pilot experiments showed that the distribution of some elements varied along length of the pine needle. Concentration variations of trace elements with the needle age and needle position within the foliage crown were also observed. This could be one way of studying the annual physiological cycle of needles. The scanning EDXRF method was compared with graphite furnace atomic absorption spectrometry (GFAAS). (authors)

Commercial Applications of X Ray Spectrometric Techniques

International Nuclear Information System (INIS)

Wegrzynek, D.

2013-01-01

In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z ≥ 10, with a few instruments capable of detecting also elements with Z ≥ 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg’s law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

X-ray Spectrometry: Basic principles

International Nuclear Information System (INIS)

Carvalho, R.M.; Teixeira, G.J.; Cardoso, R.S.; Peixoto, J.G.P.

2017-01-01

The application of X rays requires a study of its spectrum. Intrinsic difficulties of the own method and of all the instrumentation necessary for the accomplishment of this practice were related. The objective was to demonstrate the use of a commercial spectrometer using at room temperature and compare it with spectra theoretically obtained by simulation. As an initial result was that both instrumentation is compatible to be used in an X-ray beam, with and without scattering material and its theoretical data were obtained. (author)

Rare earth aerosol analysis by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Citron, I.M.; Mausner, L.F.

1982-01-01

An analytical method for the determination of four lanthanides in air filter samples is described. The method involves simultaneous quantitative determinations of La, Ce, Pr, and Nd at the microgram level by x-ray fluorescence spectrometry without chemical separation of these rare earths and without serious interferences from the dust matrices on the filters. The method has been used successfully to analyze some air filter samples collected at a rare earth processing refinery in Illinois. A description of the development of the method is given as well as the results obtained by using this method on the air filter samples. The reproducibility of the results was generally +-5%

Single-Shot Spectrometry for X-Ray Free-Electron Lasers

International Nuclear Information System (INIS)

Yabashi, Makina; Ishikawa, Tetsuya; Hastings, Jerome B.; Zolotorev, Max S.; Mimura, Hidekazu; Yumoto, Hirokatsu; Matsuyama, Satoshi; Yamauchi, Kazuto

2006-01-01

An experimental scheme to realize single-shot spectrometry for the diagnostics of x-ray free-electron lasers (XFELs) is presented. The combination of an ultraprecisely figured mirror and a perfect crystal form a simple, high-precision spectrometer that can cover an energy range from a few eV to a hundred eV with high resolution. The application of the spectrometer to determine XFEL pulse widths was investigated theoretically and experimentally. It has been shown that the present system can determine pulse widths from sub-fs to ps in a single shot even for spontaneous radiation. The system can be easily extended to even shorter pulses

Quantitative X-ray analysis of biological fluids: the microdroplet technique

International Nuclear Information System (INIS)

Roinel, N.

1988-01-01

X-ray microanalysis can be used to quantitatively determine the elemental composition of microvolumes of biological fluids. This article describes the various steps in preparation of microdroplets for analysis: The manufacturing of micropipettes, the preparation of the specimen support, the deposition of droplets on the support, shock-freezing, and lyophilization. Examples of common artifacts (incomplete rehydration prior to freezing or partial rehydration after lyophilization) are demonstrated. Analysis can be carried out either by wavelength-dispersive analysis, which is the most sensitive method, or by energy-dispersive analysis, which is more commonly available. The minimum detectable concentration is 0.05 mmol.liter-1 for 0.1-nl samples analyzed by wavelength-dispersive spectrometry and 0.5-1 mmol.liter-1 for samples analyzed by energy-dispersive spectrometry. A major problem, especially in wavelength-dispersive analysis, where high beam currents are used, is radiation damage to the specimen; in particular chloride (but also other elements) can be lost. Quantitative analysis requires the use of standard solutions with elemental concentration in the same range as those present in the specimen

Sample positioning effects in x-ray spectrometry

International Nuclear Information System (INIS)

Carpenter, D.

Instrument error due to variation in sample position in a crystal x-ray spectrometer can easily exceed the total instrumental error. Lack of reproducibility in sample position in the x-ray optics is the single largest source of system error. The factors that account for sample positioning error are described, and many of the details of flat crystal x-ray optics are discussed

Multichannel, sequential or combined X-ray spectrometry

International Nuclear Information System (INIS)

Florestan, J.

1979-01-01

X-ray spectrometer qualities and defects are evaluated for sequential and multichannel categories. Multichannel X-ray spectrometer has time-coherency advantage and its results could be more reproducible; on the other hand some spatial incoherency limits low percentage and traces applications, specially when backgrounds are very variable. In this last case, sequential X-ray spectrometer would find again great usefulness [fr

First experience with energy dispersive X-ray analysis (EDXA) in lung fibrosis

International Nuclear Information System (INIS)

Liebetrau, G.; Wiesner, B.; Strausz, J.; Zglinicki, T. von

1987-01-01

Biopsies from 68 patients suffering from interstitial lung disease were examined with regard to minerals using energy dispersive X-ray analysis. In 31 patients a higher portion of minerals or elements were found as pigments. The interpretation of these findings is difficult. If there is a occupational exposure and a reaction of the lung parenchyma the findings could be of clinical value. (author)

Comparison of two models for the X-ray dispersion produced in a Novillo Tokamak with measurements make with thermoluminescent dosemeters

International Nuclear Information System (INIS)

Flores O, A.; Castillo, A.; Barocio, S.R.; Melendez L, L.; Chavez A, E.; Cruz C, G.J.; Lopez, R.; Olayo, M.G.; Gonzalez M, P.; Azorin N, J.

1999-01-01

It was presented the results to study about the X-ray dispersion produced in the Novillo Tokamak using thermoluminescent dosemeters (DTL). The measurements were make in the equatorial plane of Tokamak, along twelve radial directions. The dispersion is observed due to the radiation interaction with walls surrounding the machine. It was proposed two types of heuristic mathematical methods for describing the X-ray dispersion, comparing them with the experimental data obtained with Dtl. The predictions of both models are adjusted well to the experimental data. (Author)

In situ determination of K, Ca, S and Si in fresh sugar cane leaves by handheld Energy Dispersive X-Ray Fluorescence Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Guerra, Marcelo B.B.; Adame, Andressa; Almeida, Eduardo de; Brasil, Marcos A.S.; Krug, Francisco J., E-mail: fjkrug@cena.usp.br [Centro de Energia Nuclear na Agricultura, Piracicaba, SP (Brazil); Schaefer, Carlos E.G.R. [Departamento de Solos, Universidade Federal de Viçosa, MG (Brazil)

2018-05-01

A portable energy dispersive X-ray fluorescence spectrometer was evaluated in the in situ analysis of fresh sugar cane leaves for real time plant nutrition diagnosis. Fresh leaf fragments (n = 10 sugar cane varieties; 20 fragments per leaf; 2 measurement sites per fragment) were irradiated and the averaged data from X-ray characteristic emission lines intensities (for K, Ca, S and Si Kα lines) were in close agreement with mass fraction data obtained by a validated comparative method. The linear correlation coefficients (r) ranged from 0.9575 for Ca to 0.9851 for Si. The obtained limits of detection were at least two-fold lower than the critical nutrient levels. Manganese can also be properly determined, but validation still requires more robust calibration models. The proposed method is a straightforward approach towards the fast evaluation of the nutritional profile of plants avoiding time-consuming steps, which involve drying, grinding, weighing, and acid digestion. (author)

Practical applications of energy dispersive X-ray microanalysis in diagnostic oral pathology

International Nuclear Information System (INIS)

Daley, T.D.; Gibson, D.

1990-01-01

Energy dispersive X-ray microanalysis is a powerful tool that can reveal the presence and relative quantities of elements in minute particles in biologic materials. Although this technique has been used in some aspects of dental research, it has rarely been applied to diagnostic oral pathology. The purpose of this paper is to inform practicing dentists and oral specialists about the diagnostic potential of this procedure by presenting three case reports. The first case involved the identification of flakes of a metallic material claimed by a 14-year-old girl to appear periodically between her mandibular molars. In the second case, a periodontist was spared a lawsuit when a freely mobile mass in the antrum of his patient was found to be a calcium-phosphorus compound not related to the periodontal packing that had been used. The third case involved the differential diagnosis of amalgam tattoo and graphite tattoo in a pigmented lesion of the hard palate mucosa. The results of the analyses were significant and indicate a role for this technique in the assessment of selected cases. Potential for wider use of energy dispersive X-ray microanalysis in diagnostic oral pathology exists as research progresses

X-ray fluorescence analysis and optical emission spectrometry of an roman mirror from Tomis, Romania

International Nuclear Information System (INIS)

Belc, M.; Bogoi, M.; Ionescu, D.; Guita, D.; Caiteanu, S.; Caiteanu, D.

2000-01-01

The miscellaneous population of Roman Empire, their diverse cultural tradition, their ability to assimilate the roman civilization spirits, had determined a permanent reassessment superimposed upon the roman contribution. Analysis was undertaken using optical emission spectrometry and non-destructive X-ray fluorescence. X-ray fluorescence analysis is a well-established method and is often used in archaeometry and other work dealing with valuable objects pertaining to the history of art and civilization. Roman mirror analysed has been found not to be made of speculum (a high tin bronze). (authors)

Applied gamma-ray spectrometry

CERN Document Server

Dams, R; Crouthamel, Carl E

1970-01-01

Applied Gamma-Ray Spectrometry covers real life application of the gamma-ray and the devices used in their experimental studies. This book is organized into 9 chapters, and starts with discussions of the various decay processes, the possible interaction mechanisms of gamma radiation with matter, and the intrinsic and extrinsic variables, which affect the observed gamma-ray and X-ray spectra. The subsequent chapters deal with the properties and fabrication of scintillation detectors, semiconductor detectors, and proportional gas counters. These chapters present some of the most widely utilized

Case Studies on Facility Characterization with X-Ray Fluorescence Spectrometry

International Nuclear Information System (INIS)

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

2008-01-01

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

Clinical applications of scanning electron microscopy and energy dispersive X-ray analysis in dermatology--an up-date

International Nuclear Information System (INIS)

Forslind, B.

1988-01-01

Dermatological papers comprising scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis data published 1983 through 1986 in international journals are reviewed, as an update to our 1984 paper on Clinical applications of scanning electron microscopy and X-ray microanalysis in dermatology. The present paper not only deals with a review of recent publications in this area but also presents the application of microincineration to hair and cryosectioned freeze-dried skin specimens. Examples of the increased contrast obtained in hair cross sections are presented and a discussion on the feasibility of microincineration at analysis of hair and skin cross sections is given. Particle probe analysis (EDX: energy dispersive X-ray analysis and PMP: proton microprobe analysis) as applied to hair and skin samples are presented with stress put on the proton probe analysis. The complementarity of EDX and PMP is demonstrated and future applications are suggested. 75 references

Design and characterization for absolute x-ray spectrometry in the 100-10,000 eV region

International Nuclear Information System (INIS)

Henke, B.L.

1986-08-01

Reviewed here are the design and characterization procedures used in our program for developing absolute x-ray spectrometry in the 100 to 10,000 eV region. Described are the selection and experimental calibration of the x-ray filters, mirror momochromators, crystal/multilayer analyzers, and the photographic (time integrating) and photoelectric (time resolving) position-sensitive detectors. Analytical response functions have been derived that characterize the energy dependence of the mirror and crystal/multilayer reflectivities and of the photographic film and photocathode sensitivities. These response functions permit rapid, small-computer reduction of the experimental spectra to absolute spectra (measured in photons per stearadian from the source for radiative transitions at indicated photon energies). Our x-ray spectrographic systems are being applied to the diagnostics of pulsed, high temperature plasma sources in laser fusion and x-ray laser research. 15 refs., 27 figs

Assembly of positioner of automated two-dimensional scan coupled to X-ray fluorescence spectrometry; Montagem de posicionador de varredura bidimensional automatizada acoplado a espectrometria de fluorescência de raios-X

Energy Technology Data Exchange (ETDEWEB)

Silva, Leonardo Santiago Melgaço

2011-07-01

This work describes the design and assembling of a prototype automated positioner two-dimensional scanning coupled to X-ray fluorescence spectrometry. The work aims to achieve a portable and easy to use, device of broad utility in the analysis of samples by X-ray fluorescence area of expertise and research. The two-dimensional scanning of the positioner is by means of two stepper motors controlled by a microcontroller PIC 16F877A, encoder and optical sensors. The user interacts with the XY table through an interface program for the Windows operating system, which communicates with the microcontroller through the serial port. The system of Fluorescence Spectroscopy incorporated into the positioner consists of a system commercially available system from the company AMPTEK, where the primary source of excitation of the sample was a source of {sup 241}Am of 59.5 KeV emissions. Resolution and accuracy of tests were performed in the XY scanning process and reproducibility of the same kit with the fluorescence spectrometry X-ray. Qualitative tests by X-ray fluorescence spectrometry in samples were performed to demonstrate the applicability and versatility of the project. It follows that the prototype illustrates a possible adequately to portable device for X-ray spectrometry of two-dimensional. (author)

Auger and depth profile analysis of synthetic crystals for dispersion of soft x-rays

International Nuclear Information System (INIS)

Rachocki, K.D.; Brown, D.R.; Springer, R.W.; Arendt, P.N.

1983-01-01

Numerous samples have been fabricated and analyzed as part of a program to produce soft x-ray dispersion elements for various laboratory applications. The majority of this work has centered around the carbon/tungsten system, although several other low-Z/high-Z pairs have been investigated. This report describes the development of certain vacuum-deposition techniques for fabricating these dispersion elements, based upon results obtained from x-ray reflectivity measurements and Auger depth-profile analysis. The composition of the films is chiefly alternating layers of tungsten carbide and carbon. Excess carbon is introduced during the deposition of the tungsten to ensure that the carbide layer is fully stoichiometric. Layer thickness ranged from approx. 5 to 30 A for the carbide and from approx. 15 to 80 A for the carbon. The reflectivity measurements were made using Fe and Al K/sub α/ at grazing incidence. The emphasis in these studies is on the application of surface-analysis results in suggesting modifications to the fabrication process and in evaluating the results such modifications have on the layer stoichiometry, continuity, and periodicity of the dispersion elements so produced

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

Science.gov (United States)

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.

X-ray fluorescence spectroscopy technology applied to the materials elementary characterization

International Nuclear Information System (INIS)

Marambio A, Cristian Gilberto.

1997-01-01

A thorough study of the different applications of energy dispersive x-ray fluorescence spectrometry is presented, using different excitation sources and measurement geometries. The adaptation of these systems focuses on the analytical solution for different sample types by studying distinct parameters such as: volume of saturation for liquid samples, inter elemental effects from the matrix and the interferences associated with the measurement reading statistical parameters: as reproducibility, precision and detection limits. The application of the technique using radioisotopic sources gave satisfactory results in the analysis of geologic samples, in analytical control of concentration processes for rare earths and for the manufacturing of fuel elements. In the case of a system with an x-ray generator two measurement geometries were studied: 45 deg geometry and total reflection. There were major results in the analysis of polymer impurities and alloy impurities, aluminums and thin semiconductor films, respectively, after non destructive in situ analysis of the material. The results show that x-ray fluorescence spectrometry is a powerful tool for analysis and process control, with prospects for the solution of analytical problems in the materials area. (author)

Photon induced x-ray fluorescence analysis using energy dispersive detector and dichotomous sampler

International Nuclear Information System (INIS)

Jaklevic, J.M.; Loo, B.W.; Goulding, F.S.

1976-01-01

Operating experience in using the photon-excited energy-dispersive x-ray fluorescence analysis system has demonstrated the applicability of this technique to large-scale air-sampling networks. This experience has shown that it is possible to perform automatic sampling and analysis of aerosol particulates at a sensitivity and accuracy more than adequate for most air pollution studies

A spectrometer for X-ray energy-dispersive diffraction using synchrotron radiation

International Nuclear Information System (INIS)

Buras, B.; Gerward, L.; Staun Olsen, J.; Steenstrup, S.

1981-10-01

The paper describes a white-beam X-ray energy dispersive diffractometer using the synchroton radiation from the DORIS ESR. The following features of the instrument are discussed: Horizontal or vertical scattering plane, collimators, sample environment, remote control of gonimeter, data acquisition, energy-sensitive detectors using small-area and large-area detector crystals, modes of operation, powder and single crystal diffraction. An example is given from a high-pressure study of YbH 2 using a diamond anvil cell. (orig./HP)

Simultaneous analysis of gaseous and particulate sulphur in the atmosphere by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Matsuda, Yatsuka; Mamuro, Tetsuo

1975-01-01

An analytical technique for the simultaneous measurements of the atmospheric concentrations of SO 2 gas and sulphur absorbed by aerosol particles has been developed. Aerosol particles are collected on membrane filter and at the same time SO 2 gas is captured on alkali impregnated filter. The sulphur content in each filter is measured by an energy dispersive X -ray fluorescence spectrometer consisting of a Si(Li) semiconductor detector connected to a multi-channel pulse height analyzer and an excitation source of 55 Fe. Two methods are acceptable for the determination of the sulphur content in impregnated filter by X-ray fluorescence analysis. In the first method X-ray fluorescence analysis is made after the collected sulphur gas diffused and distributed uniformly enough throughout the filter, and in the second method X-ray fluorescence analysis gas to be finished before the diffusion of the collected sulphur becomes appreciable. (author)

A new device for energy-dispersive x-ray fluorescence

Science.gov (United States)

Swoboda, Walter; Kanngiesser, Birgit; Beckhoff, Burkhard; Begemann, Klaus; Neuhaus, Hermann; Scheer, Jens

1991-12-01

A new measuring chamber for energy-dispersive x-ray fluorescence is presented, which allows excitation of the sample by three (commonly applied) modes: secondary target excitation, Barkla scattering, and Bragg reflection. In spite of the short distances required to obtain high intensities, the transmission of the radiator through the bulk matter of the chamber wall and the collimators could be kept negligibly small. In the case of Bragg reflection, the adjustment of all degrees of freedom of the crystal is performed independently and reproducibly under vacuum conditions. The device allows the choice of excitation mode optimized for the respective analytical problem. An experimental test using an environmental specimen shows the detection limits obtainable.

A double cell for X-ray absorption spectrometry of atomic Zn

CERN Document Server

Mihelic, A; Arcon, I; Padeznik-Gomilsek, J; Borowski, M

2002-01-01

A high-temperature cell with a double wall design has been constructed for X-ray absorption spectrometry of metal vapors. The inner cell, assembled from a corundum tube and thin plates without welding or reshaping, serves as a container of the vapor sample. It is not vacuum tight: instead, the outer tube provides inert atmosphere. Several spectra of K-edge atomic absorption of Zn were obtained in the stationary working regime below the Zn boiling point. The K-edge profile shows an extremely strong resonance and, above the continuum threshold, coexcitations of the outer electrons.

DETERMINATION OF MINERAL COMPOSITION OF ORGANIC AND CONVENTIONAL BEVERAGES BY DISPERSIVE ENERGY X-RAY FLUORESCENCE SPECTROMETRY

Directory of Open Access Journals (Sweden)

L. CONSOLI

2012-11-01

Full Text Available Fruits are natural sources of minerals whose ingestion is recommended in a balanced diet. The increasing consumption of fruit-based beverages demands the development of rapid methods to evaluate their quality parameters. X-ray fluorescence spectrometry is an analytical-nuclear technique that is gaining space in the environmental and geological fields, and has been explored modestly in the food field. The main objective of this work was to develop a methodology to determine the mineral content of fruit-based beverages by applying this technique. Beverages manufactured from organic and conventional fruit varieties were evaluated, aiming to compare their nutritional value. The research was divided into three steps: in the first step, a direct measurement of the samples was made, that is, without prior preparation; in the second, standard curves were prepared with the elements of calcium and potassium, based on the category of ‘fine samples’. Lastly, these curves were used to determine concentrations of calcium and potassium in the samples of juices and pulps prepared as ‘fine samples’. The fine sample measurements showed results more exact compared to that obtained from the direct measurements. From the data evaluated, it was not possible to attribute better nutritional quality to either the organic or conventional samples.

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-07-27

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

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

International Nuclear Information System (INIS)

Wilson, Matthew D.; Seller, Paul; Veale, Matthew C.; Connolley, Thomas; Dolbnya, Igor P.; Malandain, Andrew; Sawhney, Kawal; Grant, Patrick S.; Liotti, Enzo; Lui, Andrew

2016-01-01

A novel, “single-shot” fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200µm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 µm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 µm pinhole 13 cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm"2 with one of the 80×80 pixels imaging an area equivalent to 13µm"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.

Application of delayed X-ray spectrometry to the analysis of some rare earth elements

International Nuclear Information System (INIS)

Pillay, A.E.; Mboweni, R.C.M.

1991-01-01

The capabilities of delayed x-ray spectrometry preceded by isotope-source thermal neutron activation for the specific determination of some rare earth elements (Sm, Eu, Dy, Ho) in small powdered samples was evaluated. The feasibility study relied heavily on the low-energy sensitivity of the detector used. Detection of the delayed x-rays was achieved with a 100-mm 2 Ge detector with the ability to produce optimum photopeak-to-noise ratios. The rare earth elements were chosen on the basis of their inherent favourable nuclear properties for producing a practicable x-ray yield and on the demand for their analysis. Analytical results are presented over a range of concentrations for the elements of interest and the potential of the technique for application to their general routine analysis is discussed. Interferences from the sample matrix can be suppressed to an extent that makes the method almost independent of the matrix. This and other features make the technique a strong rival to conventional activation analysis. (author)

Morphological and chemical changes in dentin after using endodontic agents: Fourier transform Raman spectroscopy, energy-dispersive x-ray fluorescence spectrometry, and scanning electron microscopy study

Science.gov (United States)

Pascon, Fernanda Miori; Kantovitz, Kamila Rosamilia; Soares, Luís Eduardo Silva; Santo, Ana Maria do Espírito; Martin, Airton Abraha~o.; Puppin-Rontani, Regina Maria

2012-07-01

We examine the morphological and chemical changes in the pulp chamber dentin after using endodontic agents by scanning electron microscopy (SEM), Fourier transform Raman spectroscopy (FT-Raman), and micro energy-dispersive x-ray fluorescence spectrometry (μEDXRF). Thirty teeth were sectioned exposing the pulp chamber and divided by six groups (n=5): NT-no treatment; CHX-2% chlorhexidine; CHXE-2% chlorhexidine+17% EDTA E-17% EDTA; SH5-5.25% NaOCl; SH5E-5.25% NaOCl+17% EDTA. The inorganic and organic content was analyzed by FT-Raman. μEDXRF examined calcium (Ca) and phosphorus (P) content as well as Ca/P ratio. Impressions of specimens were evaluated by SEM. Data were submitted to Kruskal-Wallis and Dunn tests (pNT=SH5E>CHX>E>CHXE). CHXE and E presented the highest Ca/P ratio values compared to the other groups (p<0.05). The SEM images in the EDTA-treated groups had the highest number of open tubules. Erosion in the tubules was observed in CHX and SH5E groups. Endodontic agents change the inorganic and organic content of pulp chamber dentin. NaOCl used alone, or in association with EDTA, was the most effective agent considering chemical and morphological approaches.

X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation - Modelling, experiment, and Monte-Carlo simulation

International Nuclear Information System (INIS)

Hodoroaba, V.-D.; Radtke, M.; Vincze, L.; Rackwitz, V.; Reuter, D.

2010-01-01

X-ray scattering may contribute significantly to the spectral background of X-ray fluorescence (XRF) spectra. Based on metrological measurements carried out with a scanning electron microscope (SEM) having attached a well characterised X-ray source (polychromatic X-ray tube) and a calibrated energy dispersive X-ray spectrometer (EDS) the accuracy of a physical model for X-ray scattering is systematically evaluated for representative samples. The knowledge of the X-ray spectrometer efficiency, but also of the spectrometer response functions makes it possible to define a physical spectral background of XRF spectra. Background subtraction relying on purely mathematical procedures is state-of-the-art. The results produced by the analytical model are at least as reliable as those obtained by Monte-Carlo simulations, even without considering the very challenging contribution of multiple scattering. Special attention has been paid to Compton broadening. Relevant applications of the implementation of the analytical model presented in this paper are the prediction of the limits of detection for particular cases or the determination of the transmission of X-ray polycapillary lenses.

Characterization of nanoclays dispersion in NBR nanocomposites by X-ray diffractograms

International Nuclear Information System (INIS)

Sousa, Fabiula D.B.; Scuracchio, Carlos H.; Mantovani, Gerson L.

2009-01-01

The main objective of this work is the study of nanoclays dispersion in NBR nanocomposites by X-ray diffraction. Nitrile rubbers NBR 3330 and NBR 3350 were used, both with 33%wt of acrylonitrile and with different Mooney viscosity. The nanoclays were bentonite, organically modified montmorillonite (Cloisite 30B R ) and sodic montmorillonite. The results showed that the intercalation state of the filler had influence of both, the type of treatment at which clay was submitted and the molar mass of the polymer. (author)

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

Czech Academy of Sciences Publication Activity Database

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

2017-01-01

Roč. 140, NOV (2017), s. 161-166 ISSN 0969-806X R&D Projects: GA MŠk LM2015056 Institutional support: RVO:61389005 Keywords : Gamma-ray spectrometry * neutron activation analysis * environmental dosimetry Subject RIV: CB - Analytical Chemistry , Separation OBOR OECD: Analytical chemistry Impact factor: 1.315, year: 2016

Energy dispersive X-ray diffraction as a means to identify illicit materials: A preliminary optimisation study

Energy Technology Data Exchange (ETDEWEB)

Cook, Emily [Department of Medical Physics and Bioengineering, UCL, London WC1E 6BT (United Kingdom)]. E-mail: ecook@medphys.ucl.ac.uk; Fong, Ruby [Clinical Physics Department, St Bartholomew' s Hospital, London EC1A 7BE (United Kingdom); Horrocks, Julie [Clinical Physics Department, St Bartholomew' s Hospital, London EC1A 7BE (United Kingdom); Wilkinson, David [HOSDB, Woodcock Hill, Sandridge, Herts. AL4 9HQ (United Kingdom); Speller, Robert [Department of Medical Physics and Bioengineering, UCL, London WC1E 6BT (United Kingdom)

2007-08-15

Energy dispersive X-ray diffraction is proposed as a suitable non-destructive method to rapidly identify illicit drugs in parcels. A preliminary data set of 7 illicit drug samples and a possible cutting agent has been collected with a range of count times using a tungsten target X-ray source, a high resolution HpGe detector and a variable geometry diffraction cell. These results have been used to calibrate and train multivariate analysis software to predict the drug content in previously unseen spectra.

Energy dispersive X-ray diffraction as a means to identify illicit materials: A preliminary optimisation study

International Nuclear Information System (INIS)

Cook, Emily; Fong, Ruby; Horrocks, Julie; Wilkinson, David; Speller, Robert

2007-01-01

Energy dispersive X-ray diffraction is proposed as a suitable non-destructive method to rapidly identify illicit drugs in parcels. A preliminary data set of 7 illicit drug samples and a possible cutting agent has been collected with a range of count times using a tungsten target X-ray source, a high resolution HpGe detector and a variable geometry diffraction cell. These results have been used to calibrate and train multivariate analysis software to predict the drug content in previously unseen spectra

Precision and accuracy of multi-element analysis of aerosols using energy-dispersive x-ray fluorescence

International Nuclear Information System (INIS)

Adams, F.; Van Espen, P.

1976-01-01

Measurements have been carried out for the determination of the inherent errors of energy-dispersive X-ray fluorescence and for the evaluation of its precision and accuracy. The accuracy of the method is confirmed by independent determinations on the same samples using other analytical methods

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

International Nuclear Information System (INIS)

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

2010-01-01

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

A method to test the performance of an energy-dispersive X-ray spectrometer (EDS).

Science.gov (United States)

Hodoroaba, Vasile-Dan; Procop, Mathias

2014-10-01

A test material for routine performance evaluation of energy-dispersive X-ray spectrometers (EDS) is presented. It consists of a synthetic, thick coating of C, Al, Mn, Cu, and Zr, in an elemental composition that provides interference-free characteristic X-ray lines of similar intensities at 10 kV scanning electron microscope voltage. The EDS energy resolution at the C-K, Mn-Lα, Cu-Lα, Al-K, Zr-Lα, and Mn-Kα lines, the calibration state of the energy scale, and the Mn-Lα/Mn-Kα intensity ratio as a measure for the low-energy detection efficiency are calculated by a dedicated software package from the 10 kV spectrum. Measurements at various input count rates and processor shaping times enable an estimation of the operation conditions for which the X-ray spectrum is not yet corrupted by pile-up events. Representative examples of EDS systems characterized with the test material and the related software are presented and discussed.

A laser heating facility for energy-dispersive X-ray absorption spectroscopy

DEFF Research Database (Denmark)

Kantor, Innokenty; Marini, C.; Mathon, O.

2018-01-01

A double-sided laser heating setup for diamond anvil cells installed on the ID24 beamline of the ESRF is presented here. The setup geometry is specially adopted for the needs of energy-dispersive X-ray absorption spectroscopic (XAS) studies of materials under extreme pressure and temperature...... conditions. We illustrate the performance of the facility with a study on metallic nickel at 60 GPa. The XAS data provide the temperature of the melting onset and quantitative information on the structural parameters of the first coordination shell in the hot solid up to melting....

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

Energy Technology Data Exchange (ETDEWEB)

Wrobel, P.M. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); AGH University of Science and Technology, Faculty of Physics and Applied Computer Science, al. A. Mickiewicza 30, 30-059 Krakow (Poland); Bogovac, M. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Sghaier, H. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Institut Superieur d’Informatique et de Mathematiques de Monastir (ISIMM), Departement de technologie, 5000 Monastir (Tunisia); Leani, J.J. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); IFEG – CONICET, Facultad de Matematica Astronomia y Fisica, Universidad Nacional de Cordoba, 5000 Cordoba (Argentina); Migliori, A.; Padilla-Alvarez, R. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Czyzycki, M. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); AGH University of Science and Technology, Faculty of Physics and Applied Computer Science, al. A. Mickiewicza 30, 30-059 Krakow (Poland); Osan, J. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); Environmental Physics Department, Hungarian Academy of Sciences Centre for Energy Research, Konkoly-Thege M. út 29-33., H-1121 Budapest (Hungary); Kaiser, R.B. [Physics Section, Nuclear Science and Instrumentation Laboratory (NSIL), IAEA Laboratories, A-2444 Seibersdorf (Austria); and others

2016-10-11

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. - Highlights: • A new methodology for control of a synchrotron beamline end-station is shown. • The new control system comprises a novel binding of Tango control system with LabVIEW interface. • The reliability of the control system is demonstrated by examples of analytical applications.

Energy dispersive X-ray diffraction at high pressure in CHESS

International Nuclear Information System (INIS)

Ruoff, A.L.; Baublitz, M.A. Jr.

1981-01-01

Energy dispersive X-ray techniques were used with a diamond anvil cell in the Cornell High Energy Synchrotron Source (CHESS). It was shown that quantitative relative intensity measurement could be made when the pressure was hydrostatic and the crystals were relatively defect free. The crystal structures of the high pressure polymorphs of Ge, GaAs, GaP, and AlSb were studied. Ge exhibits the β-tetragonal structure as found by Jamieson; however, the transition pressure is 80 +- 5 kbars. GaAs exhibits an orthorhombic structure above 172 +- 7 kbars, GaP the β-Sn structure above 215 +- 8 kbars, and AlSb an orthorhombic structure above 77 +- 5 kbars. (Auth.)

Combined analysis of 1,3-benzodioxoles by crystalline sponge X-ray crystallography and laser desorption ionization mass spectrometry.

Science.gov (United States)

Hayashi, Yukako; Ohara, Kazuaki; Taki, Rika; Saeki, Tomomi; Yamaguchi, Kentaro

2018-03-12

The crystalline sponge (CS) method, which employs single-crystal X-ray diffraction to determine the structure of an analyte present as a liquid or an oil and having a low melting point, was used in combination with laser desorption ionization mass spectrometry (LDI-MS). 1,3-Benzodioxole derivatives were encapsulated in CS and their structures were determined by combining X-ray crystallography and MS. After the X-ray analysis, the CS was subjected to imaging mass spectrometry (IMS) with an LDI spiral-time-of-flight mass spectrometer (TOF-MS). The ion detection area matched the microscopic image of the encapsulated CS. In addition, the accumulated 1D mass spectra showed that fragmentation of the guest molecule (hereafter, guest) can be easily visualized without any interference from the fragment ions of CS except for two strong ion peaks derived from the tridentate ligand TPT (2,4,6-tris(4-pyridyl)-1,3,5-triazine) of the CS and its fragment. X-ray analysis clearly showed the presence of the guest as well as the π-π, CH-halogen, and CH-O interactions between the guest and the CS framework. However, some guests remained randomly diffused in the nanopores of CS. In addition, the detection limit was less than sub-pmol order based on the weight and density of CS determined by X-ray analysis. Spectroscopic data, such as UV-vis and NMR, also supported the encapsulation of the guest through the interaction between the guest and CS components. The results denote that the CS-LDI-MS method, which combines CS, X-ray analysis and LDI-MS, is effective for structure determination.

Characterization of breast tissue using energy-dispersive X-ray diffraction computed tomography

International Nuclear Information System (INIS)

Pani, S.; Cook, E.J.; Horrocks, J.A.; Jones, J.L.; Speller, R.D.

2010-01-01

A method for sample characterization using energy-dispersive X-ray diffraction computed tomography (EDXRDCT) is presented. The procedures for extracting diffraction patterns from the data and the corrections applied are discussed. The procedures were applied to the characterization of breast tissue samples, 6 mm in diameter. Comparison with histological sections of the samples confirmed the possibility of grouping the patterns into five families, corresponding to adipose tissue, fibrosis, poorly differentiated cancer, well differentiated cancer and benign tumour.

Recent trends in total reflection X-ray fluorescence spectrometry for biological applications

International Nuclear Information System (INIS)

Szoboszlai, Norbert; Polgari, Zsofia; Mihucz, Victor G.; Zaray, Gyula

2009-01-01

This review is focused on the application of total reflection X-ray fluorescence (TXRF) spectrometry in the field of biological research. In the last decade, most papers were published by authors who applied laboratory-scale TXRF equipments. The application of synchrotron radiation as excitation source (SR-TXRF) shows a slowly increasing tendency. In the cited papers the micro-, trace and multielement capability of these TXRF techniques was demonstrated in the clinical and medical laboratory practice, as well as in various plant physiological studies. For speciation of elements in biological matrices, the TXRF was used as element specific detector following an off-line separation step (e.g., thin layer chromatography, high performance liquid chromatography), however, these off-line methods are not competitive with the on-line coupled HPLC-inductively coupled plasma mass spectrometry

X-ray spectroscopy and X-ray crystallography of metalloenzymes at XFELs

International Nuclear Information System (INIS)

Yano, Junko

2016-01-01

The ultra-bright femtosecond X-ray pulses provided by X-ray Free Electron Lasers (XFELs) open capabilities for studying the structure and dynamics of a wide variety of biological and inorganic systems beyond what is possible at synchrotron sources. Although the structure and chemistry at the catalytic sites have been studied intensively in both biological and inorganic systems, a full understanding of the atomic-scale chemistry requires new approaches beyond the steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure at ambient conditions, while overcoming X-ray damage to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by using the intense and ultra-short femtosecond X-ray pulses from an XFEL, where sample is probed before it is damaged. We have developed methodology for simultaneously collecting crystallography data and X-ray emission spectra, using an energy dispersive spectrometer at ambient conditions. In addition, we have developed a way to collect metal L-edge data of dilute samples using soft X-rays at XFELs. The advantages and challenges of these methods will be described in this review. (author)

The studies of post-medieval glass by multivariate and X-ray fluorescence analysis

International Nuclear Information System (INIS)

Kierzek, J.; Kunicki-Goldfinger, J.

2002-01-01

Multivariate statistical analysis of the results obtained by energy dispersive X-ray fluorescence analysis has been used in the study of baroque vessel glasses originated from central Europe. X-ray spectrometry can be applied as a completely non-destructive, non-sampling and multi-element method. It is very useful in the studies of valuable historical artefacts. For the last years, multivariate statistical analysis has been developed as an important tool for the archaeometric purposes. Cluster, principal component and discriminant analysis were applied for the classification of the examined objects. The obtained results show that these statistical tools are very useful and complementary in the studies of historical objects. (author)

Analysis of agricultural soils by using energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Anjos, Marcelino Jose dos

2000-03-01

In this work, we describe an Energy Dispersive x-ray Fluorescence System with a x-ray tube excitation for trace analysis of environmental samples (soil). The system was used to analyze the contamination of metals in treated soils with doses of 10, 20 and 30 ton/ha of compound organic of urban garbage of the type Fertilurb and 10 ton/ha of aviary bed (manure of birds). Samples of roots and foliages of plant radishes cultivated in these soils were also analyzed. The soil samples were collected in five different depths of 0,5, 5-10, 10-20, 20-40 and 40-60 cm. The experimental set-up is composed by an OXFORD X-ray (30 kV, 50 μA and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray spectrum tube is quasi-monochromatic by using of Ti filter. Samples were prepared in pellet form with superficial density in the range of 100 mg/cm 2 . The fundamental parameter method was used in order to verify the elemental concentration. It was possible to determine the concentrations of thirteen elements: K, Ca, Ti, Mn, Fe, Cu, Zn, Br, Rb, Sr, Y, Zr and Pb in the treated soils with compounds organic. The results indicate that the values found for K, Ca, Rb, Sr, Zr and Pb are significantly above the upper confidence limits for the control soil (α = 0.05). There is a real different between these elements compared to their relationship in the control soils, (α=0,05). There is a real difference between these elements compared to their relationship in the control soils, confirming the influence of the organic compounds in the soil. (author)

Single particle transfer for quantitative analysis with total-reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Esaka, Fumitaka; Esaka, Konomi T.; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu; Watanabe, Kazuo

2006-01-01

The technique of single particle transfer was applied to quantitative analysis with total-reflection X-ray fluorescence (TXRF) spectrometry. The technique was evaluated by performing quantitative analysis of individual Cu particles with diameters between 3.9 and 13.2 μm. The direct quantitative analysis of the Cu particle transferred onto a Si carrier gave a discrepancy between measured and calculated Cu amounts due to the absorption effects of incident and fluorescent X-rays within the particle. By the correction for the absorption effects, the Cu amounts in individual particles could be determined with the deviation within 10.5%. When the Cu particles were dissolved with HNO 3 solution prior to the TXRF analysis, the deviation was improved to be within 3.8%. In this case, no correction for the absorption effects was needed for quantification

Efficient high-resolution X-ray emission spectrometry using synchrotron radiation

International Nuclear Information System (INIS)

Unterumsberger, Rainer

2015-01-01

The aim of the present work is to get access to high-resolution X-Ray Emission Spectrometry (XES) at nanoscaled materials, consisting of light elements and transition metals, by the increase of the sensitivity of a Wavelength-Dispersive Spectrometer (WDS) in the soft X-Ray range. The increase of the sensitivity was achieved by a refocusing of the incident radiation. With the increased sensitivity of the WDS, it was possible to determine the chemical species of different, nominal 100 nm thin titanium oxides. The combination of the refocusing optic and calibrated spectrometer enabled the detection and deconvolution of the L-fluorescence radiation of these nanoscaled titanium oxides. Due to the calibration of the spectrometer, a reliable determination of the transition probabilities of the titanium La- and Ll-fluorescence lines as a function of the chemical state is possible. To the best of my knowledge, the determination of the transition probabilities as a function of the chemical state in the soft X-Ray range has not been investigated yet. The quality of the refocusing was characterized using different diagnostic tools. Vertical full width at half maximum (FWHM) values of the focused beam between 10 μm to 20 μm and horizontal FWHM values between 12 μm and 25 μm could be achieved over an energy range of 180 eV to 1310 eV. Using calibrated photodiodes, it was possible to determine the absolute transmission of the used single bounce monocapillary as well as to monitor the absolute photon flux. By means of the refocusing, it was possible to increase the photon flux by a factor of 4.9 experimentally. The increase of the photon flux enables the analysis of nanoscaled materials with the used spectrometer. This could be shown based on the determination of the lower limit of detection of boron Ka and titanium La. In both cases, the lower limit of detection of 0.4 nm equivalent layer thickness was achieved (about 1.10 -7 g/cm 2 to 2.10 -7 g/cm 2 or 3.10 15 atoms/cm 2 to

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

Science.gov (United States)

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.

Determination of the structure factors of a LiF powder sample by the energy dispersive x-ray diffraction

International Nuclear Information System (INIS)

Uno, R.; Ahtee, A.; Paakkari, T.

1977-01-01

The structure factors of a LiF powder sample were determined by energy dispersive x-ray diffraction in the range 9 to 25 keV, with the use of a Si(Li) solid state detector, following the method applied on GaP. Since the absorption coefficient of LiF is small at high energy, a fraction of the incident x-rays penetrates through the sample and does not contribute to the diffraction. This effect was taken into account in the determination of the structure factors. Then the structure factors generally agree, within the limit of 5 % error, with those obtained by the usual angle dispersive method, if the penetrated part of the incident beam is less than 40 %. (author)

Comparison of two models for the X-ray dispersion produced in a Novillo Tokamak with measurements make with thermoluminescent dosemeters; Comparacion de dos modelos para la dispersion de rayos X producidos en un Novillo Tokamak con mediciones efectuadas con dosimetros termoluminiscentes

Energy Technology Data Exchange (ETDEWEB)

Flores O, A.; Castillo, A.; Barocio, S.R.; Melendez L, L.; Chavez A, E.; Cruz C, G.J.; Lopez, R.; Olayo, M.G.; Gonzalez M, P. [Instituto Nacional de Investigaciones Nucleares, 52045 Salazar, Estado de Mexico (Mexico); Azorin N, J. [Universidad Autonoma Metropolitana Iztapalapa, 09340 Mexico D.F. (Mexico)

1999-07-01

It was presented the results to study about the X-ray dispersion produced in the Novillo Tokamak using thermoluminescent dosemeters (DTL). The measurements were make in the equatorial plane of Tokamak, along twelve radial directions. The dispersion is observed due to the radiation interaction with walls surrounding the machine. It was proposed two types of heuristic mathematical methods for describing the X-ray dispersion, comparing them with the experimental data obtained with Dtl. The predictions of both models are adjusted well to the experimental data. (Author)

New software to model energy dispersive X-ray diffraction in polycrystalline materials

Energy Technology Data Exchange (ETDEWEB)

Ghammraoui, B., E-mail: bahaa.ghammraoui@cea.fr [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Tabary, J. [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Pouget, S. [CEA-INAC Sciences de la matieres, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Paulus, C.; Moulin, V.; Verger, L. [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Duvauchelle, Ph. [CNDRI-Insa Lyon, Universite de Lyon, F-69621, Villeurbanne Cedex (France)

2012-02-01

Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

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

Directory of Open Access Journals (Sweden)

Pan Liu

2017-05-01

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

Automated energy-dispersive x-ray determination of trace elements in stream sediments

International Nuclear Information System (INIS)

Hansel, J.M.; Martell, C.J.

1977-01-01

Nickel, copper, tungsten, lead, bismuth, niobium, silver, cadmium, and tin are determined in stream sediments using a computer-controlled energy-dispersive x-ray fluorescence system. The system consists of an automatic 20-position sample changer, a silicon lithium-drifted detector, a pulsed molybdenum transmission-target x-ray tube, a multichannel analyzer, and a minicomputer. Samples are analyzed as minus 325-mesh powders. A computer program positions the samples, unfolds overlapping peaks, determines peak intensities for each element, and calculates the ratio of the intensity of each peak to that of the molybdenum Kα Compton peak. Concentrations of each element are then calculated using equations obtained by analyzing prepared standards. Detection limits range from 5 ppM for silver, cadmium, lead, and bismuth to 20 ppM for niobium. The relative standard is 10 percent or less at the 100-ppM level and 20 percent at the 20-ppM level. Samples can be analyzed at the rate of sixty per day

Determination of non-ionic surfactants in technologic liquors and effluents by X-ray fluorescent spectrometry

International Nuclear Information System (INIS)

Dankowski, P.; Majda, J.

1977-01-01

The method has been worked out for determination of non-ionic surfactants in technological liquors and effluents, based on the X-ray fluorescent spectrometry with an initial concentration by means of the phosphomolybdic acid. The method is suitable for a quantitative determination of ethylene oxide adducts in a wide range of applicable concentrations, the trace-ones included. (M.Z.)

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

International Nuclear Information System (INIS)

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

2010-01-01

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% (1σ) and the results deviated from the expected values by < 4% on average.

The determination, by x-ray-fluorescence spectrometry, of gold in activated charcoal

International Nuclear Information System (INIS)

Austen, C.E.

1977-01-01

A rapid method is described for the determination of gold in activated charcoal by X-ray-fluorescence spectrometry. Compensation for matrix effects is achieved by means of platinum that is added for use as an internal standard. Calibration is achieved by use of a series of synthetic standards that are made by the spiking of barren charcoal with gold and platinum. The limit of determination is about 8 p.p.m. of gold, and the relative standard deviation is 1,2 per cent at a concentration level of 2300 p.p.m

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

International Nuclear Information System (INIS)

Necemer, Marijan; Kump, Peter; Scancar, Janez; Jacimovic, Radojko; Simcic, Jurij; Pelicon, Primoz; Budnar, Milos; Jeran, Zvonka; Pongrac, Paula; Regvar, Marjana; Vogel-Mikus, Katarina

2008-01-01

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

The X-ray spectrometry Si(Li) system and it's application in quantitative analysis of rare-earth elements

International Nuclear Information System (INIS)

Barbosa, J.B.S.

1985-11-01

The basic principles involved in Si(Li) system used in X-ray spectrometry is described. It also demonstrates its application in the energy range where the resolution is better than that characteristic of conventional spectrometers. The theoretical principles underlying the interaction between the electromagnetic radiation and matter, and a review on semiconductors are presented at first. It emphasizes the fluorescence phenomenon and the process of photon detection by semiconductor crystals whose properties and characteristics allow, in the specific case of Si-crystal, the confection of detectors with large sensitivity volume useful for X-ray spectrometry. In addition, the components of the Si(Li) system are described individually, with special attention to the operating aspects, and to the parameters affecting the quality of pulse height spectrum. Finally, the spectrometer performance is experimentally evaluated though the quantitative analyses of rare-earth element oxides (La, Ce, Pr, Nd). It should be stressed that this research indicates that the X-ray emission-transmission analysis is the most adequate method under the activation conditions provided by the spectrometer, where Am 241 emissor UPSILON of 60KeV is the photon source for the fluorescence. Therefore, the experimental work was extended in order to include all the necessary treatment. (Author) [pt

Fission products determination in high activity waste solution by wavelength dispersive X-ray fluorescence spectral interference correction by intensity ratio

International Nuclear Information System (INIS)

Sato, I.M.

1988-01-01

Fission products Se, Rb, Y, Zr, Mo, Ru, Rh, Pd, Te, Cd, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu and Gd were determined in simulated high activity radioactive waste solution by wavelength dispersive X-ray fluorescence spectrometry without chemical separation. Thin layer technique was employed for the sample preparation. For the L spectral lines, the absorption effect was verified by Rasberry-Heinrich, Lucas Tooth-Pyne and Lachance-Trail relations. This effect was quantified and corrected accordingly. The spectral interferences of Kα and/or Lα lines of Y, Zr, Mo, La, Ce, Pr, Nd, Sm, Eu and Gd elements were eliminated by the intensity ratio method. The overlapping of up to three analytical lines was corrected by applying this method. The concentration influence of the interfering element on the intensity ratio values as well the efficiency of the correction method were investigated in order to assure that no systematic or residual error, resulting from the correction, affect the actual fluorescent intensity determination. The results is compared with the data obtained from measurements of free lines of spectral interference and also with those obtained by the linear equation system. Fission products determination presented a precision in the range of 0.1 to 5.0% and an accuracy of up to ± 7.0% the results are compared with those obtained by neutron activation analysis and inductively coupled plasma - atomic emission spectrometry. Leaching data, when radioactive waste is incorporated in cement matrix, were attempted by X-ray fluorescence technique. For two years leaching period, leaching rate and diffusion coefficient data of cesium were determined. The results obtained agree with those obtained by γ-spectromety. (author) [pt

Working with Detection Limits in X-Ray and Nuclear Spectrometry

International Nuclear Information System (INIS)

Van Espen, P.

2003-01-01

Full Text: Detection limits are important in many measurement procedures. Especially in analytical work we often need to take a decision about the presence or absence of a compound, or we need to guarantee that or instrument can detect the compound. Especially in regulatory work the concept of detection limits plays a crucial role. Data acquisition in x-ray and gamma-ray spectrometry is done by counting events for a preset time; hence the fluctuations in the observed spectra are governed by Poisson (counting) statistics. This makes the calculation of detection limits in principle very easy. However it is observed that there exists a great deal of confusion concerning the definition(s) and especially concerning the practical calculation and reporting of detection limits. In this contribution a simple but rigorous treatment of the concept of detection limits will be given, emphasizing on aspects such as a-priori and a-posterior i limits and on the effect of sample blank and instrumental blank in the calculation of the true detection limit. The problem of near zero background as observed in e.g. total reflection x-ray fluorescence analysis (T-XRF) and some low level counting applications will also be discussed. In this case Poisson statistics might not be applicable, affecting the decision limits with respect to the presence of absence of a signal. Finally handling data sets that contain detection limit values next to normal measured values, the so called problem of missing data will be discussed. Some suggestions to deal with this frequently occurring situation will be given

ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

International Nuclear Information System (INIS)

Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

1987-01-01

A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

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

Science.gov (United States)

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.

The description of compton lines in energy-dispersive x-ray Fluorescence

International Nuclear Information System (INIS)

Van Gysel, Mon; Van Espen, P.J.M.

2001-01-01

Energy-Dispersive X-Ray Fluorescence (ED-XRF) is a non-destructive technique for the element analysis in a concentration range ppm - % making use of X rays up to 100 keV. Generally, two photon matter interactions occur, respectively absorption and scattering. The absorption of incident photons gives raise to characteristic lines. Scattering gives an incoherent and a coherent line. A Gaussian peak model is adequate to describe the characteristic and coherent scattered lines. Incoherent lines appear as non-Gaussian, broadened peaks. The profile of a Compton peak is complex. It depends on the geometry and the composition of the sample. Especially, when analyzing a low Z matrix; dominant scattering and multiple scattering may cause large interferences. The absence of an appropriate fitting model makes the Compton profile seen as a limiting factor in the evaluation of spectra. An accurate description of incoherent lines should improve quantitative analysis. Therefore, a suitable fitting model, making use of the expertise of non-linear least squares procedures and Monte-Carlo calculations was systematically investigated. The proposed model, containing a modified Gaussian, is tested on experimental data recorded with a HPGe detector

Simultaneous analyses of gaseous and particulate sulphur compounds in the atmosphere by x-ray fluorescence spectrometry, (1)

International Nuclear Information System (INIS)

Matsuda, Yatsuka; Mamuro, Tetsuo

1974-01-01

An analytical technique for the simultaneous measurements of the atmospheric concentrations of SO 2 gas and sulphur absorbed by aerosol particles has been developed. Aerosol particles are collected on membrane filter and at the same time SO 2 gas is captured on alkali impregnated filter. The sulphur content in each filter is measured by an energy dispersive X-ray fluorescence spectrometer consisting of a Si(Li) semiconductor detector connected to a multichannel pulse hight analyzer and an excitation source of 55 Fe. Two methods are acceptable for the determination of the sulphur content in impregnated filter by X-ray fluorescence analysis. In the first method X-ray fluorescence analysis is made after the collected sulphur has diffused and distributed uniformly enough throughout filter, and in the second method X-ray fluorescence analysis has to be finished before the diffusion of the collected sulphur becomes appreciable. (auth.)

Analysis of medieval Serbian silver coins from XIV and XV century by means of wavelength-dispersive X-ray spectrometry

Energy Technology Data Exchange (ETDEWEB)

Gržetić, Ivan [University of Belgrade, Faculty of Chemistry, Studentski trg 12-16, 11000 Belgrade (Serbia); Orlić, Jovana, E-mail: jovanaorlic@chem.bg.ac.rs [Innovation Centre of Faculty of Chemistry, University of Belgrade, Faculty of Chemistry, Studentski trg 12-16, 11000 Belgrade (Serbia); Radić, Vesna [National Museum in Belgrade, Department of Numismatic, Trg Republike 1a, 11000 Belgrade (Serbia); Radić, Milica [Innovation Centre of Faculty of Chemistry, University of Belgrade, Faculty of Chemistry, Studentski trg 12-16, 11000 Belgrade (Serbia); Ilijević, Konstantin [University of Belgrade, Faculty of Chemistry, Studentski trg 12-16, 11000 Belgrade (Serbia)

2016-01-01

X-ray fluorescence (XRF) spectrometry is known as excellent nondestructive technique for analysis of artifacts, in our case, medieval numismatic coins. Collections of 30 silver coins, owned by National Museum in Belgrade, were investigated during our research. Coins from the historical period from 1389 to 1458 belong to the reign of two Serbian rulers, Stefan Lazarević and Đurđe Branković. The aim of this study was to determine elemental composition of silver coins and to characterize alloys from which the coins were minted. The dominant elements detected in all coins were Ag, Cu, Zn and Pb. In some coins Fe, Si and S were detected as well. Results from quantitative analysis shows that the content of Ag in all investigated silver coins exceed 90%, except in two coins that were assumed to be forged. The concentration of Cu ranged from 3% to 5%, and the contents of Zn and Pb varied around 1%. Characterization of coins provided us information about raw materials and employed metallurgical processes.

Analysis of trace elements in medicinal plants with energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Ekinci, N.; Polat, R.; Budak, G.; Ekinci, R.

2004-01-01

Mankind still depend on traditional herbal medicine for the treatment of various diseases and ailments. Elemental composition and concentration of medicinal plants have been investigated by energy dispersive X-ray fluorescence. The elements present in medicinal plants are P, Cl, K, Ca, S, Al, Ti, V, Rb, Sr, Zr, Nb, Mo, In, Sn, I and Ce. The physical basis of the used analytical method, the experimental set up and the procedure of sample preparation are presented. (author)

The application of energy-dispersive X-Ray fluorescence spectrometry (EDXRF) to the analysis of ceramic glasses

International Nuclear Information System (INIS)

Ben Abdelwahed, Haifa; Reguigui, Nafaa; Ghdira, Lotfi; Khosrof, S.

2005-01-01

The measurement of energies and intensities of fluorescent X-rays emitted from a given material when atoms are bombarded with suitable projectiles like electrons, protons, α particles or photons has been successfully used for non-destructive elemental analysis in many applications, especially in the analysis of ceramic glasses. Use of radioisotopes as a source of excitation radiation in combination with high resolution semiconductor detectors in x-ray fluorescence has found wide applications in elemental analysis. A radioisotope excited X-ray fluorescence spectrometer consisting of a standard 5.45mm Si(Li) detector having a resolution of 200 eV at 5.9 keV coupled to a TRUMP-8K multichannel analyzer has been used. Tow sources of annular geometry using 10 mCi 109Cd and 10 mCi 55Fe together with PC AXIL software have been used for this study of tile-pavement glasses of ''Ksar Said'' in Tunisia. Analytical data shows that those tile pavement witch are broken in the 19th century from France (Marseille) have not the same composition of Tunisian tile pavement. Referring to our data, The kind of that analyzed glasses is of alkaline lead. we found also, through this study, the elemental compositions of different pigments (green, blue, brownish, yellow, white and red) used to color that tile-pavement glasses

The application of energy-dispersive X-Ray Fluorescence spectrometry (EDXRF) to the analysis of ceramic glasses

International Nuclear Information System (INIS)

Ben Abdelwahed, H.; Reguigui, N.; Ghidira, L.; Khosrof, S.

2005-01-01

The measurement of energies and intensities of fluorescent X-rays emitted from a given material when atoms are bombarded with suitable projectiles like electrons, protons,α particles or photons have been successfully used for non destructive elemental analysis in many applications, especially in the analysis of ceramic glasses. Use of radioisotopes as a source of excitation radiation in combination with high resolution semiconductor detectors in x-ray fluorescence has found wide applications in elemental analysis. A radioisotope excited X-ray fluorescence spectrometer consisting of a standard 5.45mm Si(Li) detector having a resolution of 200 eV at 5.9 KeV coupled to a TRUMP -8K multichannel analyser has been used. Two sources of annular geometry using 10 mCi 109 CD and 10 mCi 55 Fe together with PC AXIL software have been used for this study of tile-pavement glasses of ''Ksar Said'' in Tunisia. Analytical data shows that those tile pavements which are broken in the 19th century from France (Marseille) have not the same composition of Tunisian tile pavement. Referring to our data, the kind of that analysed glasses is of alkaline lead. We found also, through this study, the elemental compositions of different pigments (green, blue, brownish, yellow, white and red) used to color those tile-pavement glasses

Rapid analysis of molybdenum contents in molybdenum master alloys by X-ray fluorescence technique

International Nuclear Information System (INIS)

Tongkong, P.

1985-01-01

Determination of molybdenum contents in molybdenum master alloy had been performed using energy dispersive x-ray fluorescence (EDX) technique where analysis were made via standard additions and calibration curves. Comparison of EDX technique with other analyzing techniques, i.e., wavelength dispersive x-ray fluorescence, neutron activation analysis and inductive coupled plasma spectrometry, showed consistency in the results. This technique was found to yield reliable results when molybdenum contents in master alloys were in the range of 13 to 50 percent using HPGe detector or proportional counter. When the required error was set at 1%, the minimum analyzing time was found to be 30 and 60 seconds for Fe-Mo master alloys with molybdenum content of 13.54 and 49.09 percent respectively. For Al-Mo master alloys, the minimum times required were 120 and 300 seconds with molybdenum content of 15.22 and 47.26 percent respectively

Radioisotope induced energy dispersive X-ray fluorescence - a diagnostic tool in clinical science

International Nuclear Information System (INIS)

Joseph, Daisy

2010-01-01

Full text: Energy dispersive X-ray fluorescence (EDXRF) - an ideal technique for detecting trace elements in drugs have been used for analyzing drugs marked as Zn supplements (Jasad Bhasm) used for growth in children and Ayurvedic medicines containing toxic elements such as Arsenic (As) and Mercury (Hg). Folklore medicines obtained as plants extracts from Manipur plants were also analyzed for their composition. Zn supplements (Jasad Bhasm) manufactured by various manufacturers were analyzed for their trace elements besides Zn and were compared with laboratory preparations. Similarly the Ayurvedic medicines from different companies were analyzed for their metal composition. All samples in powder form were pelletized and analyzed using an X-ray spectrometer consisting of a Cd 109 radioisotope source, Si (Li) detector of resolution 170 eV at 5.9 KeV Mn X-ray, preamplifier, amplifier and a PC based multichannel analyzer. Varying amounts of trace elements were detected in Jasad Bhasm and interesting results (As and Hg) were seen in the Ayurvedic medicines in addition to other trace elements such as K,Ca,Fe,Cu and Zn. In Manipur plant extracts Sr was predominantly seen in most samples. Their levels of toxicity and significance to human health and diseases will be discussed in the remaining sections of the paper

The determination, by x-ray-fluorescence spectrometry, of gold, silver, and base metals on activated carbon

International Nuclear Information System (INIS)

Wall, G.; Jacobs, J.J.; Dixon, K.

1980-01-01

The method proposed involves ashing of the sample at a low temperature in a muffle furnace, mixing of the ash with alumina and boric acid in a Siebtechnik mill, and briquetting of the mixture. The elements are measured in the briquette by the use of x-ray fluorescence spectrometry. The detailed laboratory method is given in an appendix [af

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

International Nuclear Information System (INIS)

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

2004-01-01

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

Quantitative microanalysis in the analytical electronmicroscope using an HPGe-x ray detector

International Nuclear Information System (INIS)

Grogger, W.

1994-01-01

Energy dispersive x-ray spectrometry (EDX) is a routine method for determining the chemical composition of a sample in the analytical electronmicroscope. Since some years high purity germanium x-ray detectors (HPGe) are commercially available for use in EDX. This new type of detector offers some advantages over the commonly used Si (Li) detector: better energy resolution, better detector efficiency for high energy lines (> 30 keV) and better stability against exterior influences. For quantitative analysis one needs sensitivity factors (k-factors), which correlate the measured intensity to the concentration of a specific element. These k-factors can be calculated or determined experimentally. For a precise quantitative analysis of light elements measured k-factors are absolutely necessary. In this study k-factors were measured with an HPGe detector using standards. The accuracy of the k-factors was proved using some examples of practical relevance. Additionally some special features of the HPGe detector were examined, which lead to a better understanding of EDX spectrometry using an HPGe detector (escape lines, icing of the detector, artifacts). (author)

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

Science.gov (United States)

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.

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

Science.gov (United States)

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

2018-05-01

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

Fast and simple method for determination of fatty acid methyl esters (FAME) in biodiesel blends using X-ray spectrometry.

Science.gov (United States)

Sitko, Rafal; Zawisza, Beata; Kowalewska, Zofia; Kocot, Karina; Polowniak, Marzena

2011-09-30

The determination of fatty acid methyl esters (FAME) in diesel fuel blends is an important aspect of production and blending process as well as quality control of distribution operations. In this study, energy-dispersive X-ray fluorescence spectrometer (EDXRF) is used for the first time for determination of FAME in biodiesel blends. The principle of the method is based on intensity difference of X-ray radiation scattered from hydrocarbons and from FAME. The experiment shows that coherent and incoherent radiation, commonly applied for evaluation of the average atomic number of the sample with light matrix, cannot be applied for FAME determination. However, the application of scattered continuous radiation gives excellent correlation between FAME concentration and intensity of scattered radiation. The best results are obtained if continuum is collected in the range of energy between 10.5 and 15.0 keV for rhodium X-ray tube, operated at 35 kV. Linear relationship between the FAME concentration and the inverse of scattered continuous radiation is obtained with the correlation coefficients of 0.999. Standard deviation of measurement is ca. 0.46% (v/v) of FAME and detection limit is 1.2% (v/v) for 600 s counting time and 50% dead-time loss using Si-PIN detector. The investigation shows that crucial issue in determination of FAME in biodiesel blends using EDXRF spectrometer is the precision of measurements resulting from the counting statistics. Therefore, much better results (0.20% (v/v) standard deviation and 0.52% (v/v) detection limit) can be expected if higher intensity of primary radiation is applied and X-ray spectrum is collected by silicon drift detector of high input count rate. For concentration of FAME from 10 to 100% (v/v), the differences between reference method (Fourier transform infrared spectrometry) and the proposed method usually do not exceed 1% (v/v) of FAME. The proposed method is fast, simple and enables FAME determination in wide range of

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

International Nuclear Information System (INIS)

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

2012-01-01

Highlights: ► Chemometrics-assisted EDXRFS spectroscopy realizes direct, rapid and accurate analysis of trace bioavailable macronutrients in soils. ► The method is minimally invasive, involves little sample preparation, short analysis times and is relatively insensitive to matrix effects. ► This opens up the ability to rapidly characterize large number of samples/matrices with this method. - Abstract: 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.

A simple method to improve the quantification accuracy of energy-dispersive X-ray microanalysis

International Nuclear Information System (INIS)

Walther, T

2008-01-01

Energy-dispersive X-ray spectroscopy in a transmission electron microscope is a standard tool for chemical microanalysis and routinely provides qualitative information on the presence of all major elements above Z=5 (boron) in a sample. Spectrum quantification relies on suitable corrections for absorption and fluorescence, in particular for thick samples and soft X-rays. A brief presentation is given of an easy way to improve quantification accuracy by evaluating the intensity ratio of two measurements acquired at different detector take-off angles. As the take-off angle determines the effective sample thickness seen by the detector this method corresponds to taking two measurements from the same position at two different thicknesses, which allows to correct absorption and fluorescence more reliably. An analytical solution for determining the depth of a feature embedded in the specimen foil is also provided.

Energy dispersion of x-ray continua in the energy range 9kev to 19kev refraction on Si wafers

International Nuclear Information System (INIS)

Ebel, H.; Streli, C.; Pepponi, G.; Wobrauschek, P.

2000-01-01

Total reflection of x-rays in matter at given grazing incidence angle is characterized by the occurrence of an energy cut-off. Photons with energies greater than the cut-off energy penetrate into matter and are refracted according to a transition from the optically more dense to the optically less dense medium. Since the refractive index depends on photon energy, an energy dispersion of continuous x-radiation is observed. The present investigation is dedicated to the energy dispersion of continuous x-radiation (Mo, 45 kV) by Si wafers. Theory and experimental results are in excellent agreement. (author)

Determination of Nb in ZrO2 matrix using Wavelength Dispersive X-Ray Fluorescence (WDXRF) technique

International Nuclear Information System (INIS)

Jha, S.N.; Kapoor, S.K.; Malhotra, S.K.; Kaimal, R.; Kamat, M.J.; Sehra, J.C.

1998-09-01

A Wavelength Dispersive X-Ray Fluorescence (WDXRF) method is described for the estimation of niobium in ZrO 2 matrix in the concentration range of 0.5 to 35%. Analysis of Nb is desired during the reclamation of zirconium from Zr-2.5% Nb scrap. Zr-2.5% Nb is used in water cooled nuclear power reactors on account of high creep resistance and strength. For the reclamation of these metals from the scrap, chlorination is done to produce mixed chloride. The mixed chloride is treated to obtain individual chloride for eventually converting to respective metal. Analysis is required to ascertain purity of these metals reclaimed from the scrap. Primary x-rays from gold target x-ray tube were used to excite the K lines of Nb. A linear relation has been found between the intensity of Nb-Kα 1,2 line and concentration in the above range and the detection limit was 0.03% for 10 seconds counting time. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

2004-08-31

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

Energy-dispersive X-ray reflectivity and GID for real-time growth studies of pentacene thin films

International Nuclear Information System (INIS)

Kowarik, S.; Gerlach, A.; Leitenberger, W.; Hu, J.; Witte, G.; Woell, C.; Pietsch, U.; Schreiber, F.

2007-01-01

We use energy-dispersive X-ray reflectivity and grazing incidence diffraction (GID) to follow the growth of the crystalline organic semiconductor pentacene on silicon oxide in-situ and in real-time. The technique allows for monitoring Bragg reflections and measuring X-ray growth oscillations with a time resolution of 1 min in a wide q-range in reciprocal space extending over 0.25-0.80 A -1 , i.e. sampling a large number of Fourier components simultaneously. A quantitative analysis of growth oscillations at several q-points yields the evolution of the surface roughness, showing a marked transition from layer-by-layer growth to strong roughening after four monolayers of pentacene have been deposited

Measurement of trace elements in KH2PO4 crystals by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Ryon, R.W.; Duewer, T.I.

1981-02-01

A non-destructive method is described for the quantitative measurement of impurities in KDP (KH 2 PO 4 ) crystals. Part per million concentrations of impurities can be determined with good accuracy in about one hour of instrument time. An energy dispersive x-ray spectrometer is used. Both the crystals and the solutions from which they are grown may be analyzed

Comparison of sensitivities and detection limits between direct excitation and secondary excitation modes in energy dispersive x-ray fluorescence analysis

International Nuclear Information System (INIS)

Artz, B.E.; Short, M.A.

1976-01-01

A comparison was made between the direct tube excitation mode and the secondary target excitation mode using a Kevex 0810 energy dispersive x-ray fluorescence system. Relative sensitivities and detection limits were determined with two system configurations. The first configuration used a standard, high power, x-ray fluorescence tube to directly excite the specimen. Several x-ray tubes, including chromium, molybdenum, and tungsten, both filtered and not filtered, were employed. The second configuration consisted of using the x-ray tube to excite a secondary target which in turn excited the specimen. Appropriate targets were compared to the direct excitation results. Relative sensitivities and detection limits were determined for K-series lines for elements from magnesium to barium contained in a low atomic number matrix and in a high atomic number matrix

Electron-probe microanalysis: x-ray spectroscopy

International Nuclear Information System (INIS)

1987-01-01

The main principles on X-ray, energy and wave length dispersive spectroscopy are reviewed. In order to allow the choice of the best operating conditions, the importance of the regulation and control systems is underlined. Emission theory, X-rays nature and its interaction with matter and electrons in the matter is shown. The structure, operating procedures and necessary electronics (single channel - analysis chain) automatic-control system for the threshold-energies discrimination and the energy distribution visualization) associated to the wavelength dispersive spectroscopy are described. The focusing control, resolution, influence of chemical bonds and multilayer-structure monochromators relaled to wavelength dispersive spectroscopy are studied. Concerning the energy-dispersive spectroscopy, the detector, preamplifier, amplifier, analog-digital converter, as well as the utilization and control of the spectrometer are described. Problems and instrumental progress on energy-dispersive spectroscopy related to the electronic-noise control, charge collection and light-elements detection are discussed [fr

X-Ray Fluorescence Spectrometry. II Determination of Uranium in ores; Espectrometria de fluorescencia de Rayos X. II-Aplicacion a la determinacion de uranio en minerales

Energy Technology Data Exchange (ETDEWEB)

Bermudez Polonio, J; Crus Castillo, F. de la; Fernandez Cellini, R

1961-07-01

A method of analysis of uranium in ores by X-ray spectrometry was developed, using the internal standard technique. Strontium was found to be the most suitable internal standard for general use. A Norelco Philips X-ray fluorescent spectrometer was used in this work, equipped with a lithium fluoride crystal acting as a diffraction grating analyzer. The intensity of the uranium-L {alpha}{sub 1} spectral line is calculated and related to corresponding strontium-K{sub {alpha}} spectral line, both detected with a Scintillation Counter. (Author) 31 refs.

Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

Science.gov (United States)

Abboud, A; Kirchlechner, C; Keckes, J; Conka Nurdan, T; Send, S; Micha, J S; Ulrich, O; Hartmann, R; Strüder, L; Pietsch, U

2017-06-01

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

On the polarization mixing of X-rays

International Nuclear Information System (INIS)

Ohkawa, T.; Hashimoto, H.

1984-01-01

Relativistic quantum field theory is applied to discuss the process of interference of white X-rays and the mechanism of rotation of the polarization of X-rays in crystals. A two-photon state is studied theoretically for analyzing the mechanism of the polarization mixing. Diffracted X-ray photons are produced by two successive stages of interaction between incident X-rays and electrons in a crystal. A dispersion relation of diffracted X-rays similar to Laue's dynamic theory is shown by use of the S-matrix. A dynamical structure factor is defined on the base of Dirac's γ-matrix. (author)

The determination of Fe, Mn and Ca in sintered iron and blast-furnace slag by X-ray fluorescent analyses of energy and wave dispersion-comparison of results

International Nuclear Information System (INIS)

Dworak, B.; Gajek, Sz.

1980-01-01

The results of sintered iron and of blast-furnace slag examination obtained by X-ray fluorescent analyses of energy and of wave dispersion are compared. They show that the methods are comparable for such elements as Ca and Fe, whereas for Mn (in sinter) the X-ray fluorescent analysis of wave dispersion is less precise. (author)

Nondestructive multielement analyses of airborne particulates by combined uses of instrumental neutron activation analysis and energy dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Mamuro, Tetsuo; Matsuda, Yatsuka; Mizohata, Akira

1974-01-01

Combined uses of instrumental neutron activation analysis and energy dispersive X-ray fluorescence analysis make it possible to analyze nondestructively a considerably large number of elements in airborne particulates. We have confirmed that up to 45 elements can be analyzed without any chemical procedures for urban airborne particulate samples. As the radiation spectrometry by semiconductor detectors and the automatic data reduction by electronic computation are quite common to the two techniques, combined uses of them produce no special annoyance. Several elements can be analyzed by both of them and therefore the reliability of the analytical results can be comfirmed by comparing the data obtained by them with each other. It is noted that this confirmation can be made for the very same sample. In this article are described our experiences of multielement analyses of airborne particulates and some problems to be solved in further studies. (auth.)

Application of X-ray fluorescence (WDXRF): thickness and chemical composition determination of thin films

International Nuclear Information System (INIS)

Scapin, Valdirene de Oliveira.

2004-01-01

In this work a procedure is described for thickness and quantitative chemical composition of thin films by wavelength dispersion X-ray fluorescence (WDXRF) using Fundamental Parameters method. This method was validated according to quality assurance standard and applied sample Al, Cr, TiO2, Ni, ZrO2 (single thickness) and Ni/Cr (double thickness) on glass; Ni on steel and metallic zinc and TiO2 on metallic iron (single thickness), all the sample were prepared for physical deposition of vapor (PVD). The thickness had been compared with Absorption (FRX-A) and Rutherford Backscattering Spectrometry (RBS) methods; the result showed good efficiency of the fundamental parameters method. Sample structural characteristics analyzed by X ray diffraction (XRD) showed any influence in the thickness determinations. (author)

Scanning electron microscope/energy dispersive x ray analysis of impact residues in LDEF tray clamps

Science.gov (United States)

Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

1993-01-01

Detailed optical scanning of tray clamps is being conducted in the Facility for the Optical Inspection of Large Surfaces at JSC to locate and document impacts as small as 40 microns in diameter. Residues from selected impacts are then being characterized by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis at CNES. Results from this analysis will be the initial step to classifying projectile residues into specific sources.

Characterization of chemical elements in soil submitted to different systems use and management by energy dispersive x-ray fluorescence spectrometry (EDXRF); Caracterizacao dos niveis de elementos quimicos em solo, submetido a diferentes sistemasde uso e manejo, utilizando espectrometria de fluorescencia de raios-X por energia dispersiva (EDXRF)

Energy Technology Data Exchange (ETDEWEB)

Wastowski, Arci Dirceu; Rosa, Genesio Mario da; Cherubin, Mauricio Roberto; Rigon, Joao Paulo Gonsiorkiewicz, E-mail: wastowski@smail.ufsm.b [Universidade Federal de Santa Maria (UFSM), Frederico Westphalen, RS (Brazil). Centro de Educacao Superior Norte do Rio Grande do Sul

2010-07-01

This study aimed to evaluate the chemical elements levels in soil, submitted to different management systems and use by the Energy Dispersive X-Ray Fluorescence Spectrometry - EDXRF. The systems were T1 - agroforestry (SAF), T2 - native field (CN), T3 - native forest (NM), T4 - tillage forest (PF); T5 - conventional tillage system (SPC) and T6 - system tillage (NT). Samples were collected at 0-10 and 10-20 cm, dried and ground for analysis in EDX-720. The soil showed no difference in the average concentrations of chemical elements analyzed in the profiles, but the systems presented different concentrations of metal elements, and T3 had the highest K, Ca and Zn at 0-10 cm and higher contents of K, Ca, Cu, Zn and Mn in the layer of 10-20 cm. (author)

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

International Nuclear Information System (INIS)

Nielson, K.K.

1977-07-01

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

Investigations of the phase transition in V3O5 using energy dispersive X-ray diffraction and synchrotron radiation white beam X-ray topography

International Nuclear Information System (INIS)

Asbrink, S.; Gerward, L.; Staun Olsen, J.

1985-01-01

The reversible first order phase transition in V 3 O 5 at T t =155 0 C has been studied using a specially constructed oven, where the temperature can be kept constant within a few hundredths of a degree for several hours. Energy dispersive diffraction measurements have beem made in a temperature region around the phase transition with the fixed crystal method and the θ/2θ scanning method. White beam X-ray topographs have been obtained from the same crystal in the same temperature region using synchrotron radiation. The integrated intensities of the strong h 0 0 reflections show anomalies that are correlated with the corresponding X-ray topographs. Thus, an unexpected increase of crystal perfection is observed a few hundredths of a degree below T t . The energy dependence of the intensity maximum at T t for strong reflections has been determined and semi-quantitatively explained on the basis of extinction theory. (orig.)

Application of low power X-ray tubes in geology

International Nuclear Information System (INIS)

Massalski, J.M.; Zaraska, W.

1981-01-01

Low power X-ray tubes with transmission anodes for X-ray fluorescence analysis with energy dispersion were elaborated. Paper contains experimental results of application of X-ray tubes in the apparatus for nondestructive measurements of the concentration of some elements in borehole cores. (author)

Resonant inelastic x-ray scattering studies of elementary excitations

NARCIS (Netherlands)

Ament, Lucas Johannes Peter (Luuk)

2010-01-01

Resonant Inelastic X-ray Scattering (RIXS) is an X-ray in, X-ray out technique that enables one to study the dispersion of excitations in solids. In this thesis, we investigated how various elementary excitations of transition metal oxides show up in RIXS spectra.

TX 2000: total reflection and 45o energy dispersive x-ray fluorescence spectrometer

International Nuclear Information System (INIS)

Pasti, F.; Torboli, A.; Valdes, M.

2000-01-01

This equipment, developed by Ital Structures, combines two kinds of energy dispersive X-ray fluorescence techniques, the first using total reflection geometry and the second conventional 45 o geometry. The equipment is completely controlled by a PC and to reach the condition of total reflection is very easy because it is enough to load the file with the right position for the corresponding energy. In this apparatus we used an x-ray tube with an alloy anode of Mo/W with a long fine focus at 2200 W. To monochromatize the x-ray beam while choosing, for example, the Mo K alpha or W L alpha or a piece of white spectrum of 33 keV, we use a highly reflective multilayer made of Si/W with 2d = 45.5 A o . The detector used in the equipment is a lithium drifted silicon detector (Si(Li)) with an excellent energy resolution of 135 eV at 5.9 keV and 1000 cps. We developed two programs written in Windows 95, 98 and NT for a 32 bit microprocessor. The first one is called TYACQ32 and has the following functions: first, complete control of the hardware, second automatic alignment of the TX 2000 spectrometer and third acquisition of spectra. The second program is EDXRF32. This is a program to accomplish spectrum and quantitative analysis for TXRF and EDXRF 45 o degrees analysis. (author)

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

Science.gov (United States)

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

2010-03-01

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

Determination of nickel in chloralkali electrolysis brines by X-ray fluorescence spectrometry on a membrane filter

International Nuclear Information System (INIS)

Andrade, L.L.; Minzl, E.

1984-01-01

X-ray fluorescence spectrometry after ammonium pyrrolidinedithiocarbamate (APDC) preconcentration is proposed for the determination of nickel in chloralkali electrolysis brines. The optimum conditions for the precipitation target tube, peak intensity, background, analysing crystal, counters and exposure time were investigated. The method was applied to chloralkali brines of evaporite salts (halite, sylvinite, carnallite and tachhydrite), sodium, potassium and magnesium salts, explored in Sergipe (Brazil), by Petrobras-Mineracao S.A.(Author) [pt

Capacity of X-ray fluorescence analysis

International Nuclear Information System (INIS)

Wobrauschek, P.; Kregsamer, P.

1997-01-01

X-Ray fluorescence analysis (XRF) is a powerful analytical tool for the qualitative and quantitative determination of chemical elements in a sample. Two different detection principles are accepted widely: wavelength dispersive and energy dispersive. Various sources for XRF are discussed: X-ray tubes, accelerators for particle induced XRF, radioactive isotopes, and the use of synchrotron radiation. Applications include environmental, technical, medical, fine art, and forensic studies. Due to the demands of research and application special techniques like total reflection XRF (TXRF) were developed with ultimately achievable detection limits in the femtogram region. The elements detectable by XRF range from Be to U. (author)

Quantitative analysis of the sediments from the Solimoes/Amazonas river flood plain using energy dispersive x-ray fluorescence technique

International Nuclear Information System (INIS)

Carneiro, Ana E.V.

1995-01-01

A methodology for quantitative analysis of geological, biological and environmental samples with a high fraction of light elements (atomic number less than 13), using energy dispersive X-ray fluorescence technique with radioisotopic excitation, is proposed. The proposed procedure is based on the method of Fundamental Parameters for analytical elements (≥->13 evaluation, and coherent and incoherent scattered radiation for the quantitation of the light fraction of the matrix. In the order to obtain the characteristic X-ray of the elements in the Mn to Zr range a Cd-109 annular radioactive source (1,70 GBq) was used, and for Al to CR, Fe-55 (o,74 GBq). For the X-ray detection a Si (Li) detector coupled to a multichannel emulation card was employed. The characteristic X-ray net intensity as well as the coherent and incoherent scattered intensities were obtained by using the AXL software for spectrum analysis. (author). 89 refs., 37 figs., 32 tabs

Low-energy X-ray and gamma spectrometry using silicon photodiodes; Espectrometria de raios X e gama de baixa energia utilizando fotodiodos de silicio

Energy Technology Data Exchange (ETDEWEB)

Silva, Iran Jose Oliveira da

2000-08-01

The use of semiconductor detectors for radiation detection has increased in recent years due to advantages they present in comparison to other types of detectors. As the working principle of commercially available photodiodes is similar to the semiconductor detector, this study was carried out to evaluate the use of Si photodiodes for low energy x-ray and gamma spectrometry. The photodiodes investigated were SFH-205, SFH-206, BPW-34 and XRA-50 which have the following characteristics: active area of 0,07 cm{sup 2} and 0,25 cm{sup 2}, thickness of the depletion ranging from 100 to 200 {mu}m and junction capacitance of 72 pF. The photodiode was polarized with a reverse bias and connected to a charge sensitive pre-amplifier, followed by a amplifier and multichannel pulse analyzer. Standard radiation source used in this experiment were {sup 241} Am, {sup 109} Cd, {sup 57} Co and {sup 133} Ba. The X-ray fluorescence of lead and silver were also measured through K- and L-lines. All the measurements were made with the photodiodes at room temperature.The results show that the responses of the photodiodes very linear by the x-ray energy and that the energy resolution in FWHM varied between 1.9 keV and 4.4 keV for peaks corresponding to 11.9 keV to 59 keV. The BPW-34 showed the best energy resolution and the lower dark current. The full-energy peak efficiency was also determined and it was observed that the peak efficiency decreases rapidly above 50 keV. The resolution and efficiency are similar to the values obtained with other semiconductor detectors, evidencing that the photodiodes used in that study can be used as a good performance detector for low energy X-ray and gamma spectrometry. (author)

Automated three-dimensional X-ray analysis using a dual-beam FIB

International Nuclear Information System (INIS)

Schaffer, Miroslava; Wagner, Julian; Schaffer, Bernhard; Schmied, Mario; Mulders, Hans

2007-01-01

We present a fully automated method for three-dimensional (3D) elemental analysis demonstrated using a ceramic sample of chemistry (Ca)MgTiO x . The specimen is serially sectioned by a focused ion beam (FIB) microscope, and energy-dispersive X-ray spectrometry (EDXS) is used for elemental analysis of each cross-section created. A 3D elemental model is reconstructed from the stack of two-dimensional (2D) data. This work concentrates on issues arising from process automation, the large sample volume of approximately 17x17x10 μm 3 , and the insulating nature of the specimen. A new routine for post-acquisition data correction of different drift effects is demonstrated. Furthermore, it is shown that EDXS data may be erroneous for specimens containing voids, and that back-scattered electron images have to be used to correct for these errors

Elements in normal and cirrhotic human liver. Potassium, iron, copper, zinc and bromine measured by X-ray fluorescence spectrometry

DEFF Research Database (Denmark)

Laursen, J.; Milman, N.; Leth, Peter Mygind

1990-01-01

Various elements (K, Fe, Cu, Zn, Br) were measured by X-ray flourescence spectrometry in cellular and connective tissue fractions of normal and cirrhotic liver samples obtained at autopsy. Normal livers: 32 subjects (16 males, 16 females) median age 69 years. Cirrhotic livers: 14 subjects (13 mal...

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

Energy Technology Data Exchange (ETDEWEB)

Kaniu, M.I., E-mail: ikaniu@uonbi.ac.ke [Institute of Nuclear Science and Technology, University of Nairobi, P.O. Box 30197-00100 Nairobi (Kenya); Angeyo, K.H. [Department of Physics, University of Nairobi, P.O. Box 30197-00100 Nairobi (Kenya); Mwala, A.K. [Department of Land Resource Management and Agricultural Technology, University of Nairobi, P.O. Box 30197-00100 Nairobi (Kenya); Mangala, M.J. [Institute of Nuclear Science and Technology, University of Nairobi, P.O. Box 30197-00100 Nairobi (Kenya)

2012-06-04

Highlights: Black-Right-Pointing-Pointer Chemometrics-assisted EDXRFS spectroscopy realizes direct, rapid and accurate analysis of trace bioavailable macronutrients in soils. Black-Right-Pointing-Pointer The method is minimally invasive, involves little sample preparation, short analysis times and is relatively insensitive to matrix effects. Black-Right-Pointing-Pointer This opens up the ability to rapidly characterize large number of samples/matrices with this method. - Abstract: 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 {sup 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{sup 2} > 0.9) and low SEP (0.01% for N and Na, 0.05% for C, 0.08% for Mg and 1.98 {mu}g g{sup -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

Elemental analysis by portable Ag and Rh X-ray sources of a Namban type folding screen

Energy Technology Data Exchange (ETDEWEB)

Pessanha, Sofia [Centro de Física Atómica da Universidade de Lisboa, Av. Professor Gama Pinto, 2 1649-003 Lisboa (Portugal); Le Gac, Agnès [Centro de Física Atómica da Universidade de Lisboa, Av. Professor Gama Pinto, 2 1649-003 Lisboa (Portugal); Departamento de Conservação e Restauro, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Quinta da Torre, 2829-516 Caparica (Portugal); Madeira, Teresa Isabel; Guerra, Mauro [Centro de Física Atómica da Universidade de Lisboa, Av. Professor Gama Pinto, 2 1649-003 Lisboa (Portugal); Carvalho, Maria Luisa, E-mail: luisa@cii.fc.ul.pt [Centro de Física Atómica da Universidade de Lisboa, Av. Professor Gama Pinto, 2 1649-003 Lisboa (Portugal)

2013-08-15

This work focuses on the characterization of the materials used in a Japanese Namban type folding screen. Namban is the art style inspired by the arrival of the southern barbarians or Nambanjin to Japan in 1543, and the commercial trade then initiated. Energy dispersive X ray spectrometry (EDXRF) was used and complemented with Raman spectroscopy. The unexpected aspect about this screen concerns the brownish–grey color over which the characters stand instead of the usual golden color obtained by gilding. To better assess the elemental composition of the background and, most importantly, conclude about the presence of precious metals, an X-ray tube with Rh anode was used supporting the results obtained with the Ag one.

Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method.

Science.gov (United States)

Lu, Ping; Moya, Jaime M; Yuan, Renliang; Zuo, Jian Min

2018-03-01

The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maxima (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K + L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. With increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping. Published by Elsevier B.V.

Solar X-ray bursts

International Nuclear Information System (INIS)

Urnov, A.M.

1980-01-01

In the popular form the consideration is given to the modern state tasks and results of X-ray spectrometry of solar bursts. The operation of X-ray spectroheliograph is described. Results of spectral and polarization measurings of X-ray radiation of one powerful solar burst are presented. The conclusion has been drawn that in the process of burst development three characteristic stages may be distingwished: 1) the initial phase; just in this period processes which lead to observed consequences-electromagnetic and corpuscular radiation are born; 2) the impulse phase, or the phase of maximum, is characterised by sharp increase of radiation flux. During this phase the main energy content emanates and some volumes of plasma warm up to high temperatures; 3) the phase of burst damping, during which plasma cools and reverts to the initial condition

Development of multilayer optics for X-ray broadband spectrometry of plasma emission

International Nuclear Information System (INIS)

Emprin, Benoit

2014-01-01

Within the framework of the research on inertial confinement fusion, the 'Commissariat a l'energie atomique et aux energies alternatives' has studied and implemented an absolute calibrated time-Resolved broadband soft x-Ray spectrometer, called 'Diagnostic de Mesure du rayonnement X'. This diagnostic, composed of 20 measurement channels, measures the emitted radiant power from a laser created plasma in the range from 50 eV to 20 keV. We have developed additional measurement channels to obtain redundancy and an improvement in measurement accuracy. The principle of these new channels is based on an original concept to obtain spectral bounded flat-Responses. Two channels have been developed for the 2 - 4 keV and 4 - 6 keV spectral ranges, using aperiodic multilayer mirrors made at the 'Laboratoire Charles Fabry' with Cr/Sc and Ni/W/SiC/W layers respectively. These mirrors were characterized at synchrotron radiation facilities and integrated into the spectrometer. The two new channels were used during laser-Plasma experimental campaigns at the OMEGA laser facility in Rochester (USA). This allowed us to determine directly the radiant power with only one measurement within a certain spectral band, and with a better precision when compared with using standard channels. The results, in good agreement with the standard measurement channels, allowed us to validate the use of aperiodic multilayer mirrors for X-Ray broadband spectrometry. (author) [fr

Summary of existing information on gamma-ray and X-ray attenuation coefficients of solutions

DEFF Research Database (Denmark)

Singh, K.; Gerward, Leif

2002-01-01

Accurate values of X-ray and gamma-ray attenuation coefficients of different chemicals are required in spectrometry as well as in many other scientific, engineering and medical disciplines involving photon radiation. The current state of knowledge of experimental and theoretical gamma-ray and X-r......-ray attenuation coefficients in aqueous solutions of salts is presented and exemplified by recent work. The results presented provide a basis for studying X-ray and gamma-ray photon interactions with ions in solution (hydrated ions) rather than ion compounds in solid form....

In situ characterization of ancient plaster and pigments on tomb walls in Egypt using energy dispersive X-ray diffraction and fluorescence

International Nuclear Information System (INIS)

Uda, M.

2004-01-01

A portable type of energy dispersive X-ray diffraction and fluorescence (ED-XRDF) spectrometer was developed, whose operation mode is completely different from that of an X-ray diffractometer commercially available. The former is operated in energy dispersive mode but the latter in angle dispersive mode. The performance of the ED-XRDF spectrometer was tested in the field, i.e. in the tomb of Amenhotep III, built in 1364 B.C. or earlier in Egypt. The crystal structure and chemical composition of ancient plaster and pigments were successfully determined in the field using the spectrometer. The same areas investigated by the ED-XRDF spectrometer were also examined with an optical microscope. The plaster is found to be composed of anhydrite, calcite and quartz. White and yellow pigments were identified as huntite and orpiment, respectively. Egyptian blue and goethite were found in the green colored parts

Calibration of energy dispersive x-ray spectrometers for analysis of thin environmental samples

International Nuclear Information System (INIS)

Giauque, R.D.; Garrett, R.B.; Goda, L.Y.

1976-01-01

Four separate techniques for calibrating energy dispersive x-ray spectrometers are described. They include the use of (1) individual evaporated elemental thin-film standards, (2) nebulized multielement standard solution deposits to determine relative elemental sensitivity factors, (3) a semi-empirical approach to calculate relative elemental sensitivity factors, and (4) thick pure element disks. The first three techniques are applicable for a broad range of elements. The utilization of nebulized multielement standard solution deposits, along with an evaporated single element thin-film standard for absolute system calibration, is the most accurate method of the calibration techniques described

Broad-band hard X-ray reflectors

DEFF Research Database (Denmark)

Joensen, K.D.; Gorenstein, P.; Hoghoj, P.

1997-01-01

Interest in optics for hard X-ray broad-band application is growing. In this paper, we compare the hard X-ray (20-100 keV) reflectivity obtained with an energy-dispersive reflectometer, of a standard commercial gold thin-film with that of a 600 bilayer W/Si X-ray supermirror. The reflectivity...... of the multilayer is found to agree extraordinarily well with theory (assuming an interface roughness of 4.5 Angstrom), while the agreement for the gold film is less, The overall performance of the supermirror is superior to that of gold, extending the band of reflection at least a factor of 2.8 beyond...... that of the gold, Various other design options are discussed, and we conclude that continued interest in the X-ray supermirror for broad-band hard X-ray applications is warranted....

High-Performance X-ray Detection in a New Analytical Electron Microscope

Science.gov (United States)

Lyman, C. E.; Goldstein, J. I.; Williams, D. B.; Ackland, D. W.; vonHarrach, S.; Nicholls, A. W.; Statham, P. J.

1994-01-01

X-ray detection by energy-dispersive spectrometry in the analytical electron microscope (AEM) is often limited by low collected X-ray intensity (P), modest peak-to-background (P/B) ratios, and limitations on total counting time (tau) due to specimen drift and contamination. A new AFM has been designed with maximization of P. P/B, and tau as the primary considerations. Maximization of P has been accomplished by employing a field-emission electron gun, X-ray detectors with high collection angles, high-speed beam blanking to allow only one photon into the detector at a time, and simultaneous collection from two detectors. P/B has been maximized by reducing extraneous background signals generated at the specimen holder, the polepieces and the detector collimator. The maximum practical tau has been increased by reducing specimen contamination and employing electronic drift correction. Performance improvments have been measured using the NIST standard Cr thin film. The 0-3 steradian solid angle of X-ray collection is the highest value available. The beam blanking scheme for X-ray detection provides 3-4 times greater throughput of X-rays at high count rates into a recorded spectrum than normal systems employing pulse-pileup rejection circuits. Simultaneous X-ray collection from two detectors allows the highest X-ray intensity yet recorded to be collected from the NIST Cr thin film. The measured P/B of 6300 is the highest level recorded for an AEM. In addition to collected X-ray intensity (cps/nA) and P/B measured on the standard Cr film, the product of these can be used as a figure-of-merit to evaluate instruments. Estimated minimum mass fraction (MMF) for Cr measured on the standard NIST Cr thin film is also proposed as a figure-of-merit for comparing X-ray detection in AEMs. Determinations here of the MMF of Cr detectable show at least a threefold improvement over previous instruments.

Aluminum-containing dense deposits of the glomerular basement membrane: identification by energy dispersive X-ray analysis

International Nuclear Information System (INIS)

Smith, D.M. Jr.; Pitcock, J.A.; Murphy, W.M.

1982-01-01

Heavy metals, including gold, mercury, lead, bismuth, and cadmium, have the potential to cause renal disease. With the development of X-ray microanalysis, these heavy metals can now be identified in tissue deposits. This report describes a case of renal failure, probably related to dysproteinemia, in which granular, electron-opaque dense deposits were present in the glomerular basement membranes. Energy dispersive X-ray analysis demonstrated that these dense deposits contained aluminum. An analysis of this patient's history in relation to the current knowledge of aluminum metabolism suggests that the aluminum deposition occurred secondary to previous glomerular injury. This case emphasizes the need to utilize heavy metal identification technology whenever granular, electron-opaque dense deposits are identified and represents, to our knowledge, the first study to document aluminum deposits within the glomerular basement membrane of humans

Charged particle induced energy dispersive X-ray analysis

International Nuclear Information System (INIS)

Johansson, S.A.E.

1979-01-01

This review article deals with the X-ray emission induced by heavy, charged particles and the use of this process as an analytical method (PIXE). The physical processes involved, X-ray emission and the various reactions contributing to the background, are described in some detail. The sensitivity is calculated theoretically and the results compared with practical experience. A discussion is given on how the sensitivity can be optimized. The experimental arrangements are described and the various technical problems discussed. The analytical procedure, especially the sample preparation, is described in considerable detail. A number of typical practical applications are discussed. (author)

Determination of carbon in natural freshwater biofilms with total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Ovari, M.; Streli, C.; Wobrauschek, P.; Zaray, Gy.

2009-01-01

There is a growing interest in determination of low Z elements, i.e., carbon to phosphorus, in biological samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as 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). Biofilms can be used for biomonioring purposes in the aquatic environment. Besides the trace metals, especially the determination of the carbon content is important for the better understanding of the early stage of biofilm formation. For this, an ATI low Z spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a Si(Li) detector with ultra thin window was used. Biofilms were grown on two different artificial supports (granite and plexiglass), freeze dried, suspended in high purity water and analyzed. As an internal standard the natural titanium content of the biofilms was used. The accuracy of the method was checked by total carbon measurement using a combusting carbon analyzer.

Determination of carbon in natural freshwater biofilms with total reflection X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ovari, M. [Department of Analytical Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary)], E-mail: ovari@chem.elte.hu; Streli, C.; Wobrauschek, P. [Atominstitut of the Austrian Universities, TU-Wien, Stadionallee 2, A-1020, Wien (Austria); Zaray, Gy. [Department of Analytical Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary); Cooperative Research Centre of Environmental Chemistry, Eoetvoes University, Budapest, H-1117, Budapest, Pazmany Peter stny. 1/a. (Hungary)

2009-08-15

There is a growing interest in determination of low Z elements, i.e., carbon to phosphorus, in biological samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as 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). Biofilms can be used for biomonioring purposes in the aquatic environment. Besides the trace metals, especially the determination of the carbon content is important for the better understanding of the early stage of biofilm formation. For this, an ATI low Z spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a Si(Li) detector with ultra thin window was used. Biofilms were grown on two different artificial supports (granite and plexiglass), freeze dried, suspended in high purity water and analyzed. As an internal standard the natural titanium content of the biofilms was used. The accuracy of the method was checked by total carbon measurement using a combusting carbon analyzer.

Chlorine determination in (U, Pu)C fuel by total reflection X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Misra, Nand Lal; Dhara, Sangita; Mudher, Khush Dev Singh; Aggarwal, Suresh K.; Thakur, Uday Kumar; Shah, Dipti; Sawant, R.M.; Ramakumar, K.L.

2007-01-01

A Total Reflection X-ray Fluorescence (TXRF) method for the determination of chlorine in (U,Pu)C has been developed. The method involves calibration of the instrument with standard solutions and validation of TXRF determination of chlorine using synthetic standard solutions. Cl K α line excited with W L α source was used for TXRF determinations of chlorine. Chlorine present in trace amounts in (U,Pu)C samples was first separated by pyro hydrolysis. The evolved chlorine, in form of HCl, was collected in 5 mM NaOH solution. This solution was analyzed for chlorine by Total Reflection X-ray Fluorescence Spectrometry using cobalt as an internal standard. The TXRF detection limit of chlorine was found to be 3.6 pg with sample size of 30 μL. In order to assess the applicability of TXRF method for chlorine determinations in other nuclear materials, one U 3 O 8 trace element standard was also analyzed for chlorine in similar way. The precision of the method was found to be 25% (1 σ) at ng level in most of the cases. (author)

X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

International Nuclear Information System (INIS)

Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J.; Dziadowicz, M.; Kopeć, E.; Majewska, U.; Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I.; Wudarczyk-Moćko, J.; Góźdź, S.

2015-01-01

A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

Energy Technology Data Exchange (ETDEWEB)

Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Dziadowicz, M.; Kopeć, E. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Majewska, U. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Wudarczyk-Moćko, J. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Góźdź, S. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Institute of Public Health, Jan Kochanowski University, IX Wieków Kielc 19, 25-317 Kielce (Poland)

2015-12-01

A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

Application of X-ray emission techniques for monitoring environmental pollution

International Nuclear Information System (INIS)

Bernasconi, G.; Danesi, P.R.; Dargie, M.; Haselberger, N.; Markowicz, A.; Tajani, A.

1997-01-01

X-ray emission techniques are versatile and powerful methods used for multielement non-destructive analysis. They include X-ray fluorescence (XRF), particle induced X-ray emission (PIXE), scanning electron microscopy combined with X-ray spectrometry and electron probe microanalysis (EPMA). Since many years the IAEA has utilised and promoted these techniques for the analysis of environmental, biological and geological samples. In this paper recent progress at our laboratory in selected aspects related to the application of X-ray emission techniques is briefly overviewed. (authors)

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

International Nuclear Information System (INIS)

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

2010-01-01

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

Interim report task 3: immobilization process/equipment testing - task 3.4: non-destructive evaluation appendices part 2 of 2 to Lawrence Livermore National Laboratory under contract b345772

International Nuclear Information System (INIS)

Stewart, M W A; Vance, E R; Day, R A; Lumpkin, G R

2000-01-01

Nine appendices are included: Appendix A - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-2 - Th/U-doped baseline ceramic; Appendix B - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-4 - Th/U-doped baseline + impurities ceramic; Appendix C - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-10 - Th/U-doped zirconolite-rich ceramic; Appendix D - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-12 - Th/U-doped brannerite-rich ceramic; Appendix E - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-14 - Th/U-doped nominally 10 % perovskite ceramic; Appendix F - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-16 - Th/U-doped ∼ 10 % phosphate-doped ceramic;Appendix G - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-1 - Pu/U-doped baseline ceramic ;Appendix H - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition A-7 and B3-13 - Pu/U-doped baseline + impurities ceramics; and, Appendix I - Scanning electron micrographs, energy dispersive x-ray spectrometry image analysis and x-ray diffraction results for samples of composition B1-13 - Pu/U-doped nominally 10% perovskite ceramic

Determination of C and O and other elements by alpha-induced X-ray energy spectrometry

International Nuclear Information System (INIS)

Henningsen, W.P.; Schaetzler, H.P.; Kuehn, W.

1978-01-01

X-ray energy spectrometry combined with alpha-excitation by means of radionuclides, especially Po-210, has been found as a versatile tool for multielement analysis. Down to Z = 6 (carbon) qualitative and quantitative measurements have been carried out with energy resolution good enough to separate adjacent elements. Thereby errors and lowest detectable concentrations were in the region of one percent. By utilizing M- and L-X-radiation the set of detectable elements can be opened to high atomic numbers. As an example with special regard to environmental research cadmium in organic matrix was measured down to 100 ppm without any preconcentration. Much lower detection limits might be reached by appropriate measures. (orig.) [de

Using the scanning electron microscope and energy dispersive x-ray spectrometer to do mineral identification and compositional point counting on unconsolidated marine sediments

International Nuclear Information System (INIS)

Robson, S.H.

1982-01-01

This paper describes a rapid and accurate method of point-counting sands and silt-size in unconsolidated open-ocean sediments. As traditional techniques for this operation cannot be employed on the fine-grained material which frequently forms the bulk of deep sea marine sediments, an alternative method has been sought. The method described makes use of equipment known as QUANTEX-RAY comprising a computerised data acquisition and reduction system designed for use in X-ray energy spectrometry and used in conjunction with a scanning electron microscope (SEM). Grains that cannot be identified by their visual morphology in the scanning electron microscope are analysed by X-ray spectrometry. Spectra are acquired in 200 seconds or less and processed by a sequence of software routines under semi-automatic control producing a listing of oxide concentrations as the final result. Each user must customize the control programme and operating conditions to suit his requirements

Single photon energy dispersive x-ray diffraction

International Nuclear Information System (INIS)

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S.; Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H.; Tang, Henry

2014-01-01

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored

Single photon energy dispersive x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S. [Department of Physics, Clarendon Laboratory, University of Oxford, Parks Road, Oxford OX1 3PU (United Kingdom); Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H. [Lawrence Livermore National Laboratory, Livermore, California 94551 (United States); Tang, Henry [Department of Earth and Planetary Science, University of California Berkeley, Berkeley, California 94720 (United States)

2014-03-15

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.

Development of analytical software for semi-quantitative analysis of x-ray spectrum acquired from energy-dispersive spectrometer

International Nuclear Information System (INIS)

Karim, A.; Rana, M.A.; Qamar, R.; Latif, A; Ahmad, M.; Farooq, M.A.; Ahmad, Z.

2003-12-01

Software package for elemental analysis for X-ray spectrum obtained from Energy Dispersive Spectrometer (EDS) attached with Scanning Electron Microscope (SEM) has been developed: A Personal Computer Analyzer card PCA-800 is used to acquire data from the EDS. This spectrum is obtained in binary format, which is transformed into ASCII format using PCAII card software. The program is modular in construction and coded using Microsoft's QUICKBASIC compiler linker. Energy line library containing all lines of elements is created for analysis of acquired characteristic X-ray spectrum. Two techniques of peak identification are provided. Statistical tools are employed for smoothing of a curve and for computing area under the curve. Elemental concentration is calculated in weight % and in atomic. (author)

Characterization of black volcanites from the Limay river basin, Patagonia, Argentina, using energy dispersive X-ray fluorescence spectrometry: an aid to infer human group mobility

International Nuclear Information System (INIS)

Palacios, O.M.

2013-01-01

The investigation of hunter-gatherers archaeological sites in the Limay river basin, Patagonia, Argentina, raised questions concerning the lithic technology. The chemical characterization of artifacts, rocks and possible sources of provenances could help to elucidate the hunter-gatherer mobility. In three archaeological sites-Rincon Chico 2 (RCh2/87; 14 C 710 ± 60 BP), Cueva Traful I (CTI; 14 C 9430 ± 230 BP) and Casa de Piedra de Ortega (CPO; 14 C 2840 ± 80 BP), tools and debitage or discarded flakes made in black volcanic rock have been found. Nearby an extensive rock outcrop of black volcanite, Paso Limay quarry (CPL), with similar characteristics was located. Samples coming from these four sites were analyzed by energy dispersive X-ray fluorescence spectrometry. This characterization allowed the geochemical classification of the lithic material and to correlate the samples with the suspected source after a previous statistical analysis. The majority of the samples were classified as dacites and rhyolites. Only samples coming from CPO site, the closest place to CPL were made exclusively with the quarry rocks. A set of five samples from RCh2/87 and two samples from CTI appear to have same chemical composition as CPL in spite of this site is placed in the opposite bank of the Limay river suggesting that hunter-gatherers could accede to the quarry, eventually. Finally, only a set of five samples coming from RCh2/87 and CTI do not group with the quarry. This fact evidences the existence of secondary sources of supply. The information of this research allowed inferring ancient human mobility patterns in the region. (author)

Tables of X-ray absorption corrections and dispersion corrections: The new versus the old

International Nuclear Information System (INIS)

Creagh, D.

1990-01-01

This paper compared the data on X-ray absorption coefficients calculated by Creagh and Hubbell and tabulated in International Tables for Crystallography, vol. C, ed. A.J.C. Wilson (1990) section 4.2.4 with empirical (Saloman, Hubbell and Scofield, At. Data and Nucl. Data Tables 38 (1988) 1, and semi-empirical (Hubbell, McMaster, Kerr Del Grande and Mallett, in: International Tables for Crystallography, vol. IV, eds. Ibers and Hamilton (Kynoch, Birmingham, 1974)) tabulations as well as the renormalized relativistic Dirac-Hartree-Fock calculations of Scofield. It also makes comparisons of the real part of the dispersion correction f'(ω,0), with theoretical data sets (Cromer and Liberman, J. Chem. Phys. 53 (1970) 1891, and Acta Crystallogr. A37 (1981)267; Wang, Phys. Rev. A34 (1986) 636; Kissel, in: Workshop Report on New Dimensions in X-ray Scattering, CONF-870459 (Livermore, 1987) p. 9) and data collected using a variety of experimental techniques. In both cases the data is shown to give improved self-consistency and agreement with experimental. (orig./HSI)

Analysis for iodide in groundwater by x-ray fluorescence spectrometry after collection as silver iodide on activated charcoal

International Nuclear Information System (INIS)

Howe, P.T.

1980-01-01

The report describes the determination of microgram quantities of iodide in water by X-ray fluorescence spectrometry. The iodide is concentrated by precipitation as silver iodide on activated charcoal. If a 60-mL sample is available, a concentration of 0.12 mg/L can be detected. Precision (2σ) at the 1-mg/L level is +- 0.08 mg/L. (auth)

Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

International Nuclear Information System (INIS)

Hoefler, H.; Streli, C.; Wobrauschek, P.; Ovari, M.; Zaray, Gy.

2006-01-01

Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm 2 active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors

Analysis of low Z elements in various environmental samples with total reflection X-ray fluorescence (TXRF) spectrometry

Energy Technology Data Exchange (ETDEWEB)

Hoefler, H. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria); Streli, C. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria)]. E-mail: streli@ati.ac.at; Wobrauschek, P. [Atominstitut of the Austrian Universities, TU-Wien, A-1020 Vienna (Austria); Ovari, M. [Eoetvoes University, Institute of Chemistry, H-1117, Budapest, Pazmany P. stny 1/a. (Hungary); Zaray, Gy. [Eoetvoes University, Institute of Chemistry, H-1117, Budapest, Pazmany P. stny 1/a. (Hungary)

2006-11-15

Recently there is a growing interest in low Z elements such as carbon, oxygen up to sulphur and phosphorus in biological specimen. Total reflection X-ray fluorescence (TXRF) spectrometry is a suitable technique demanding only very small amounts of sample. On the other side, the detection of low Z elements is a critical point of this analytical technique. Besides other effects, self absorption may occur in the samples, because of the low energy of the fluorescence radiation. The calibration curves might be not linear any longer. To investigate this issue water samples and samples from human cerebrospinal fluid were used to examine absorption effects. The linearity of calibration curves in dependence of sample mass was investigated to verify the validity of the thin film approximation. The special requirements to the experimental setup for low Z energy dispersive fluorescence analysis were met by using the Atominstitute's TXRF vacuum chamber. This spectrometer is equipped with a Cr-anode X-ray tube, a multilayer monochromator and a SiLi detector with 30 mm{sup 2} active area and with an ultrathin entrance window. Other object on this study are biofilms, living on all subaqueous surfaces, consisting of bacteria, algae and fungi embedded in their extracellular polymeric substances (EPS). Many trace elements from the water are bound in the biofilm. Thus, the biofilm is a useful indicator for polluting elements. For biomonitoring purposes not only the polluting elements but also the formation and growth rate of the biofilm are important. Biofilms were directly grown on TXRF reflectors. Their major elements and C-masses correlated to the cultivation time were investigated. These measured masses were related to the area seen by the detector, which was experimentally determined. Homogeneity of the biofilms was checked by measuring various sample positions on the reflectors.

Nondestructive, energy-dispersive x-ray fluorescence analysis of product-stream concentrations from reprocessed LWR fuels

International Nuclear Information System (INIS)

Camp, D.C.; Ruhter, W.D.; Benjamin, S.

1979-01-01

Energy-dispersive x-ray fluorescence analysis can be used for quantitative on-line monitoring of the product concentrations in single- or dual-element process streams in a reprocessing plant. The 122-keV gamma ray from 57 Co is used to excite the K x-rays of uranium and/or plutonium in nitric acid solution streams. A collimated HPGe detector is used to measure the excited x-ray intensities. Net solution radioactivity may be measured by eclipsing the exciting radiation, or by measuring it simultaneously with a second detector. The technique is nondestructive and noninvasive, and is easily adapted directly to pipes containing the solution of interest. The dynamic range of the technique extends from below 1 to 500 g/l. Measurement times depend on concentration, but better than 1% counting statistics can be obtained in 100 s for 400 g/l concentrations, and in 1000 s for as little as 10 g/l. Calibration accuracies of 0.3% or better over the entire dynamic range can be achieved easily using carefully prepared standards. Computer-based analysis equipment allows concentration changes in flowing streams to be dynamically monitored. Changes in acid normality of the stream will affect the concentration determined, hence it must also be determined by measuring the intensity of a transmitted 57 Co beam. The computer/disk-based pulse-height analysis system allows all necessary calculations to be done on-line. Experimental requirements for an in-plant installation or a test and evaluation are discussed

The analysis, by a fusion procedure and X-ray-fluorescence spectrometry, of silicates and slags

International Nuclear Information System (INIS)

Jacobs, J.J.; Balaes, A.M.E.

1980-01-01

A glass-disc fusion method is described for the analysis, by X-ray-fluorescence spectrometry, of slags and silicate materials. The data are corrected for detector dead time and short-term instrumental drift. Corrections are made for matrix variations by use of the Lachange-Traill mathematical model, and the results are processed on a mini-computer, an iterative procedure being used in the solving of the simultaneous equations. As the alpha-correction coefficients of the Lachange-Traill model are not truly constant, a modified version of the model is proposed [af

Composition measurement in substitutionally disordered materials by atomic resolution energy dispersive X-ray spectroscopy in scanning transmission electron microscopy.

Science.gov (United States)

Chen, Z; Taplin, D J; Weyland, M; Allen, L J; Findlay, S D

2017-05-01

The increasing use of energy dispersive X-ray spectroscopy in atomic resolution scanning transmission electron microscopy invites the question of whether its success in precision composition determination at lower magnifications can be replicated in the atomic resolution regime. In this paper, we explore, through simulation, the prospects for composition measurement via the model system of Al x Ga 1-x As, discussing the approximations used in the modelling, the variability in the signal due to changes in configuration at constant composition, and the ability to distinguish between different compositions. Results are presented in such a way that the number of X-ray counts, and thus the expected variation due to counting statistics, can be gauged for a range of operating conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

X-ray dosimetry in mammography for W/Mo and Mo/Mo combinations utilizing Compton spectrometry

International Nuclear Information System (INIS)

Almeida Junior, Jose N.; Terini, Ricardo A.; Herdade, Silvio B.; Furquim, Tania A.C.

2009-01-01

Mean Glandular Dose (MGD) cannot be measured directly in mammography equipment. Therefore, methods based on Compton spectrometry are alternatives to evaluate dose distributions in a standard breast phantom, as well as mean glandular dose. In this work, a CdTe detector was used for the spectrometry measurements of radiation scattered by compton effect, at nearly 90, by a PMMA cylinder. For this, the reconstruction of primary beam spectra from the scattered ones has been made using Klein-Nishina theory and Compton formalism, followed by a determination of incident air kerma, absorbed dose values in the breast phantom and, finally, MGD. Incident and attenuated X-ray spectra and depth-dose distributions in a BR-12 phantom have been determined and are presented for the mammography range (28 to 35kV), showing good agreement with previous literature data, obtained with TLD. (author)

Heavy ion recoil spectrometry of Si{sub x}Ge{sub 1-x} thin films

Energy Technology Data Exchange (ETDEWEB)

Walker, S.R.; Johnston, P.N.; Bubb, I.F. [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D.D.; Dytlewski, N. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia); Hult, M.; Whitlow, H.J. [Lund Institute of Technology, Solvegatan (Sweden). Department of Nuclear Physics; Zaring, C.; Oestling, M. [Royal Inst. of Tech., Stockholm (Sweden). Dept. of Solid State Electronics

1993-12-31

Mass and energy dispersive recoil spectrometry employing 77 MeV {sup 127}I ions from ANTARES (FN Tandem) facility at Lucas Heights has been used to examine the isotopic composition of samples of Si{sub x}Ge{sub 1-x} grown at the Australian National University by Electron Beam Evaporation (EBE). The recoiling target nuclei were analysed by a Time Of Flight and Energy (TOF-E) detector telescope composed of two timing pickoff detectors and a surface barrier (energy) detector. From the time of flight and energy, the ion mass can be determined and individual depth distributions for each element can be obtained. Recoil spectrometry has shown the presence of oxygen in the Si{sub x}Ge{sub 1-x} layer and has enabled the separate determination of energy spectra for individual elements. 9 refs., 3 figs.

Heavy ion recoil spectrometry of Si{sub x}Ge{sub 1-x} thin films

Energy Technology Data Exchange (ETDEWEB)

Walker, S R; Johnston, P N; Bubb, I F [Royal Melbourne Inst. of Tech., VIC (Australia); Cohen, D D; Dytlewski, N [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia); Hult, M; Whitlow, H J [Lund Institute of Technology, Solvegatan (Sweden). Department of Nuclear Physics; Zaring, C; Oestling, M [Royal Inst. of Tech., Stockholm (Sweden). Dept. of Solid State Electronics

1994-12-31

Mass and energy dispersive recoil spectrometry employing 77 MeV {sup 127}I ions from ANTARES (FN Tandem) facility at Lucas Heights has been used to examine the isotopic composition of samples of Si{sub x}Ge{sub 1-x} grown at the Australian National University by Electron Beam Evaporation (EBE). The recoiling target nuclei were analysed by a Time Of Flight and Energy (TOF-E) detector telescope composed of two timing pickoff detectors and a surface barrier (energy) detector. From the time of flight and energy, the ion mass can be determined and individual depth distributions for each element can be obtained. Recoil spectrometry has shown the presence of oxygen in the Si{sub x}Ge{sub 1-x} layer and has enabled the separate determination of energy spectra for individual elements. 9 refs., 3 figs.

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

Science.gov (United States)

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...

Determination of the Effective Detector Area of an Energy-Dispersive X-Ray Spectrometer at the Scanning Electron Microscope Using Experimental and Theoretical X-Ray Emission Yields.

Science.gov (United States)

Procop, Mathias; Hodoroaba, Vasile-Dan; Terborg, Ralf; Berger, Dirk

2016-12-01

A method is proposed to determine the effective detector area for energy-dispersive X-ray spectrometers (EDS). Nowadays, detectors are available for a wide range of nominal areas ranging from 10 up to 150 mm2. However, it remains in most cases unknown whether this nominal area coincides with the "net active sensor area" that should be given according to the related standard ISO 15632, or with any other area of the detector device. Moreover, the specific geometry of EDS installation may further reduce a given detector area. The proposed method can be applied to most scanning electron microscope/EDS configurations. The basic idea consists in a comparison of the measured count rate with the count rate resulting from known X-ray yields of copper, titanium, or silicon. The method was successfully tested on three detectors with known effective area and applied further to seven spectrometers from different manufacturers. In most cases the method gave an effective area smaller than the area given in the detector description.

Determination of impurities in magnesium and aluminium by X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Roca, M.; Diaz-Guerra, J.P.

1979-01-01

The determination of traces of Al, Cr, Cu, Fe, Mn, Ni, Pb, Si and of Bi, Cr, Cu, Fe, Ga, Mg, Mn, Ni, Pb, Si, Sn, Ti, V and Zn in samples of magnesium and aluminium, respectively, by means of X-ray fluorescence spectrometry, are studied. An automatic sequential spectrometer with an on-line computer for the treatment of data has been employed. The most suitable measurement parameters have been chosen for each element in order to achieve detection limits to a few p.p.m. For magnesium in the form of drillings the analyses are performed with satisfactory results for most impurities by pressing the samples into briquettes and employing metallic discs as standards. Correction methods for the spectral interferences of Ti on V, and V on Cr have been applied. (author)

X-ray diffraction studies of NbTe 2 single crystal

Indian Academy of Sciences (India)

The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size ...

The Determination of Composite Elements in Zircaloy-2 by X-Ray Fluorescence and Emission Spectrometry Method

International Nuclear Information System (INIS)

Dian Anggraini; Rosika Kriswarini; Yusuf N

2007-01-01

Analysis of composing elements in zircaloy-2 has been done by Emission Spectrometry method and X-Ray Fluorescence (XRF). The aim of the analysis is to verify conformity between composing elements in zircaloy-2 and the material certificate. Spectrometry Emission method has higher sensitivity in element determination of a material than that of XRF method, so can be estimated that emission spectrometry method has higher accuracy than that of XRF method. The result of qualitative analysis by Emission Spectrometry indicate that the composing elements in zircaloy-2 were Sn, Cr and Ni. However, the qualitative analysis result by XRF method indicated that the composing elements in zircaloy 2 were Sn, Cr, Ni and Fe. Fe element can not be analysed by Emission Spectrometry method because Emission Spectrometer did not equipped with Fe detector. The quantitative analysis result of the composing elements in the material with both methods showed that Sn, Cr and Ni concentration of zircaloy 2 existed in concentration ranges of the material certificate. Result of statistical test (F and t-test) of analysis result of both methods can be used for analyzing composing elements in zircaloy 2. Emission Spectrometry method was more sensitive and accurate for determining Cr and Ni element in zircaloy 2 than that of emission Spectrometry method but both methods had same accuracy. The precision of measurement of Sn, Cr and Ni element using XRF method was better than that of Emission spectrometry method. (author)

Improvements on Low Level Activity Gamma Measurements and X-ray Spectrometry at the CEA-MADERE Measurement Platform

OpenAIRE

Sergeyeva Victoria; Domergue Christophe; Destouches Christophe; Girard Jean Michel; Philibert Hervé; Bonora Jonathan; Thiollay Nicolas; Lyoussi Abdallah

2016-01-01

The CEA MADERE platform (Measurement Applied to DosimEtry in REactors) is a part of the Instrumentation Sensors and Dosimetry Laboratory (LDCI). This facility is dedicated to the specific activity measurements of solid and radioactive samples using Gamma and X-ray spectrometry. MADERE is a high-performance facility devoted to neutron dosimetry for experimental programs performed in CEA and for the irradiation surveillance programmes of PWR vessels. The MADERE platform is engaged in a continuo...

Processing and quantification of x-ray energy dispersive spectra in the Analytical Electron Microscope

International Nuclear Information System (INIS)

Zaluzec, N.J.

1988-08-01

Spectral processing in x-ray energy dispersive spectroscopy deals with the extraction of characteristic signals from experimental data. In this text, the four basic procedures for this methodology are reviewed and their limitations outlined. Quantification, on the other hand, deals with the interpretation of the information obtained from spectral processing. Here the limitations are for the most part instrumental in nature. The prospects of higher voltage operation does not, in theory, present any new problems and may in fact prove to be more desirable assuming that electron damage effects do not preclude analysis. 28 refs., 6 figs

X-ray observations of planetary nebulae

International Nuclear Information System (INIS)

Apparao, K.M.V.; Tarafdar, S.P.

1990-01-01

The Einstein satellite was used to observe 19 planetary nebulae and X-ray emission was detected from four planetary nebulae. The EXOSAT satellite observed 12 planetary nebulae and five new sources were detected. An Einstein HRI observation shows that NGC 246 is a point source, implying that the X-rays are from the central star. Most of the detected planetary nebulae are old and the X-rays are observed during the later stage of planetary nebulae/central star evolution, when the nebula has dispersed sufficiently and/or when the central star gets old and the heavy elements in the atmosphere settle down due to gravitation. However in two cases where the central star is sufficiently luminous X-rays were observed, even though they were young nebulae; the X-radiation ionizes the nebula to a degree, to allow negligible absorption in the nebula. Temperature T x is obtained using X-ray flux and optical magnitude and assuming the spectrum is blackbody. T x agrees with Zanstra temperature obtained from optical Helium lines. (author)

Quantitative analysis without standards using local peak-to-background ratios with the energy dispersive X-ray microanalyzer EDR-184

International Nuclear Information System (INIS)

Eggert, F.; Heckel, J.

1986-01-01

The method realized in program QMA-184 of the energy dispersive X-Ray-Microanalyzer EDR-184 for quantitative spectra analyzing of bulk materials by using local peak-to-background ratios is described in detail. The authors demonstrate efficiency and limitations of the used method by discussion of experimental results. (author)

The analysis of anode sludges by x-ray-fluorescence spectrometry

International Nuclear Information System (INIS)

Austen, C.E.; Wall, G.J.

1978-01-01

A method is described for the analysis, by X-ray-fluorescence spectrometry, of anode sludges for the determination of antimony, bismuth, copper, iron, lead, nickel, selenium, silver, tellurium, tin, and zinc. The preparation of the samples involves fusion with a flux of barium peroxide and lithium hydroxide, and with dichromium trioxide as the internal standard, in a zirconium or vitreous-carbon crucible and casting of the melt in an aluminium mould; the fused disc so formed is then pulverized and briquetted to form pellets. Calibration curves, which are straight lines for all the elemets determined because the flux contains a heavy absorber, are established by measurement of pellets prepared from standard anode sludges, pure metals, compounds of the metals, or any combination of these materials. The precision of the results varies between 2 and 15 per cent relative standard deviation, depending on the concentration of the element being determined. The accuracy of the results is comparable with that obtained by wet-chemical methods. The laboratory method is given in an appendix

Depth profiling: RBS versus energy-dispersive X-ray imaging using scanning transmission electron microscopy

International Nuclear Information System (INIS)

Markwitz, Andreas

2000-01-01

Rutherford backscattering spectrometry (RBS) is known to be one of the techniques ideal for analysis of thin films. Elemental concentrations of matrix components and impurities can be investigated as well as depth profiles of almost each element of the periodic table. Best of all, RBS has both a high sensitivity and a high depth resolution, and is a non-destructive analysis technique that does not require specific sample preparation. Solid-state samples are mounted without preparation inside a high-vacuum analysis chamber. However, depth-related interpretation of elemental depth profiles requires the material density of the specimen and stopping power values to be taken into consideration. In many cases, these parameters can be estimated with sufficient precision. However, the assumed density can be inaccurate for depth scales in the nanometer range. For example, in the case of Ge nanoclusters in 500 nm thick SiO 2 layers, uncertainty is related to the actual position of a very thin Ge nanocluster band. Energy-dispersive X-ray emission (EDX) spectroscopy, using a high-resolution scanning transmission electron microscope (STEM) can assist in removing this uncertainty. By preparing a thin section of the specimen, EDX can be used to identify the position of the Ge nanocluster band very precisely, by correlating the Ge profile with the depth profiles of silicon and oxygen. However, extraction of the concentration profiles from STEM-EDX spectra is in general not straightforward. Therefore, a combination of the two very different analysis techniques is often the best and only successful way to extract high-resolution concentration profiles

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

International Nuclear Information System (INIS)

Ridolfi, S

2012-01-01

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

Application of decision tree algorithm for identification of rock forming minerals using energy dispersive spectrometry

Science.gov (United States)

Akkaş, Efe; Çubukçu, H. Evren; Artuner, Harun

2014-05-01

Rapid and automated mineral identification is compulsory in certain applications concerning natural rocks. Among all microscopic and spectrometric methods, energy dispersive X-ray spectrometers (EDS) integrated with scanning electron microscopes produce rapid information with reliable chemical data. Although obtaining elemental data with EDS analyses is fast and easy by the help of improving technology, it is rather challenging to perform accurate and rapid identification considering the large quantity of minerals in a rock sample with varying dimensions ranging between nanometer to centimeter. Furthermore, the physical properties of the specimen (roughness, thickness, electrical conductivity, position in the instrument etc.) and the incident electron beam (accelerating voltage, beam current, spot size etc.) control the produced characteristic X-ray, which in turn affect the elemental analyses. In order to minimize the effects of these physical constraints and develop an automated mineral identification system, a rule induction paradigm has been applied to energy dispersive spectral data. Decision tree classifiers divide training data sets into subclasses using generated rules or decisions and thereby it produces classification or recognition associated with these data sets. A number of thinsections prepared from rock samples with suitable mineralogy have been investigated and a preliminary 12 distinct mineral groups (olivine, orthopyroxene, clinopyroxene, apatite, amphibole, plagioclase, K- feldspar, zircon, magnetite, titanomagnetite, biotite, quartz), comprised mostly of silicates and oxides, have been selected. Energy dispersive spectral data for each group, consisting of 240 reference and 200 test analyses, have been acquired under various, non-standard, physical and electrical conditions. The reference X-Ray data have been used to assign the spectral distribution of elements to the specified mineral groups. Consequently, the test data have been analyzed using

Energy dispersive X-ray analysis in the electron microscope

CERN Document Server

Bell, DC

2003-01-01

This book provides an in-depth description of x-ray microanalysis in the electron microscope. It is sufficiently detailed to ensure that novices will understand the nuances of high-quality EDX analysis. Includes information about hardware design as well as the physics of x-ray generation, absorption and detection, and most post-detection data processing. Details on electron optics and electron probe formation allow the novice to make sensible adjustments to the electron microscope in order to set up a system which optimises analysis. It also helps the reader determine which microanalytical me

Interim report on task 1.2: near equilibrium processing requirements part 2 of 2 appendices to Lawrence Livermore National Laboratory for contract b345772

International Nuclear Information System (INIS)

Stewart, M W A; Vance, E R; Day, R A; Brownscombe, A

1999-01-01

Ten appendices are included: Appendix A - Copies of fabrication work instructions, consisting mostly of micrographs; Appendix B - X-ray diffraction results of the samples from task 2, which contains a list of the raw data files; Appendix C - Scanning electron micrographs and energy dispersive x-ray spectrometry results for samples of composition B1-2 - Th/U-doped baseline ceramic; Appendix D - Scanning electron micrographs and energy dispersive x-ray spectrometry results for samples of composition B1-4 - TH/U-doped baseline + impurities ceramic; Appendix E - Scanning electron micrographs and energy dispersive x-ray spectrometry results for samples of composition B1-10 - Th/U-doped zirconolite-rich ceramic; Appendix F - Scanning electron micrographs and energy dispersive x-ray spectrometry results for samples of composition B1-12 - Th/U-doped brannerite-rich ceramic; Appendix G - Scanning electron micrographs and energy dispersive x-ray spectrometry results for samples of composition B1-14 - Th/U-doped, nominally ∼ 10 % perovskite ceramic; Appendix H - Scanning eleCtron micrographs and energy dispersive x-ray spectrometry results for samples of composition B1-16 - Th/U-doped, nominally ∼ 10 % phosphate ceramic; Appendix I - Scanning electron micrographs and energy dispersive x-ray spectrometry results for the plutonium-doped samples; and Appendix J - Scanning electron micrographs and energy dispersive x-ray spectrometry results of samples sintered in 3.7 % hydrogen in argon

Fundamental parameters method for quantitative energy dispersive x-ray fluorescence analysis

International Nuclear Information System (INIS)

Demirel, H.; Zararsiz, A.

1986-01-01

In this study, the requirement of the standart material in photon excited energy distributed X-ray fluorescence analysis has been removed. The interaction of X-rays with matter has been taken into account. A computer program has been developed by using the fundamental parameters of X-ray fluorescence technique and the spectral intensity 'K' of pure elements at saturation thickness has been obtained. For experimental purpose a convenient source-target-detector geometry has been designed. In order to excite the samples,Cd-109 radioisotope source has been used. The peak intensities has been obtained in a vacum chamber by counting the emitted X-rays. The calculation of concentration has been performed for double mixed samples correcting the effects of absorption and enchancement factors. The results were in conformity with their certificate values. (author)

Determination of rubidium and strontium in geological materials by X-Ray fluorescence spectrometry

International Nuclear Information System (INIS)

Roca, M.

1979-01-01

In order to determine whole-rock ages by the Rb/Sr procedure, an X-ray fluorescence spectrometry method for the determination of both elements has been developed. The samples are pressed into boric acid backed and ringed pellets with this material as a binding agent. Matrix corrections are made following the determination od the mass absorption coefficients, based on the intensity of the Compton-scattered peak of MoKα. or MoKβ 1 .3. The U. S. Geological Survey granodiorite GSP-1 is used as a reference standard. Spectral-line interferences have been carefully studied and the empirical correction factors determined. A BASIC language program for calculating the Rb and Sr concentrations and the Rb/Sr ratios has been written. (Author) 7 refs

In-situ studies of the recrystallization process of CuInS2 thin films by energy dispersive X-ray diffraction

International Nuclear Information System (INIS)

Thomas, D.; Mainz, R.; Rodriguez-Alvarez, H.; Marsen, B.; Abou-Ras, D.; Klaus, M.; Genzel, Ch.; Schock, H.-W.

2011-01-01

Recrystallization processes during the sulfurization of CuInS 2 (CIS) thin films have been studied in-situ using energy dispersive X-ray diffraction (EDXRD) with synchrotron radiation. In order to observe the recrystallization isolated from other reactions occurring during film growth, Cu-poor, small grained CIS layers covered with CuS on top were heated in a vacuum chamber equipped with windows for synchrotron radiation in order to analyze the grain growth mechanism within the CIS layer. In-situ monitoring of the grain size based on diffraction line profile analysis of the CIS-112 reflection was utilized to interrupt the recrystallization process at different points. Ex-situ studies by electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX) performed on samples of intermediate recrystallization states reveal that during the heat treatment Cu and In interdiffuse inside the layer indicating the importance of the mobility of these two elements during CuInS 2 grain growth.

Spatially resolved quantification of agrochemicals on plant surfaces using energy dispersive X-ray microanalysis.

Science.gov (United States)

Hunsche, Mauricio; Noga, Georg

2009-12-01

In the present study the principle of energy dispersive X-ray microanalysis (EDX), i.e. the detection of elements based on their characteristic X-rays, was used to localise and quantify organic and inorganic pesticides on enzymatically isolated fruit cuticles. Pesticides could be discriminated from the plant surface because of their distinctive elemental composition. Findings confirm the close relation between net intensity (NI) and area covered by the active ingredient (AI area). Using wide and narrow concentration ranges of glyphosate and glufosinate, respectively, results showed that quantification of AI requires the selection of appropriate regression equations while considering NI, peak-to-background (P/B) ratio, and AI area. The use of selected internal standards (ISs) such as Ca(NO(3))(2) improved the accuracy of the quantification slightly but led to the formation of particular, non-typical microstructured deposits. The suitability of SEM-EDX as a general technique to quantify pesticides was evaluated additionally on 14 agrochemicals applied at diluted or regular concentration. Among the pesticides tested, spatial localisation and quantification of AI amount could be done for inorganic copper and sulfur as well for the organic agrochemicals glyphosate, glufosinate, bromoxynil and mancozeb. (c) 2009 Society of Chemical Industry.

Tables of X-ray absorption corrections and dispersion corrections: the new versus the old

Science.gov (United States)

Creagh, Dudley

1990-11-01

This paper compares the data on X-ray absorption coefficients calculated by Creagh and Hubbell and tabulated in International Tables for Crystallography, vol. C, ed. A.J.C. Wilson (1990) section 4.2.4 [1] with empirical (Saloman, Hubbell and Scofield, At. Data and Nucl. Data Tables 38 (1988) 1, [6]) and semi-empirical (Hubbell, McMaster, Kerr Del Grande and Mallett, in: International Tables for Crystallography, vol. IV, eds. Ibers and Hamilton (Kynoch, Birmingham, 1974) [2]) tabulations as well as the renormalized relativistic Dirac-Hartree-Fock calculations of Scofield [6]. It also makes comparisons of the real part of the dispersion correction ƒ‧(ω, 0) and tabulated in ref. [1], with theoretical data sets (Cromer and Liberman, J. Chem. Phys. 53 (1970) 1891, and Acta Crystallogr. A37 (1981) 267 [4,5]; Wang, Phys. Rev. A34 (1986) 636 [85]; Kissel, in: Workshop Report on New Dimensions in X-ray Scattering, CONF-870459 (Livermore, 1987) p. 9 [86]) and data collected using a variety of experimental techniques. In both cases the data tabulated in ref. [1] is shown to give improved self-consistency and agreement with experiment.

Efficient isotope ratio analysis of uranium particles in swipe samples by total-reflection x-ray fluorescence spectrometry and secondary ion mass spectrometry

International Nuclear Information System (INIS)

Esaka, Fumitaka; Watanabe, Kazuo; Fukuyama, Hiroyasu; Onodera, Takashi; Esaka, Konomi T.; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu

2004-01-01

A new particle recovery method and a sensitive screening method were developed for subsequent isotope ratio analysis of uranium particles in safeguards swipe samples. The particles in the swipe sample were recovered onto a carrier by means of vacuum suction-impact collection method. When grease coating was applied to the carrier, the recovery efficiency was improved to 48±9%, which is superior to that of conventionally-used ultrasoneration method. Prior to isotope ratio analysis with secondary ion mass spectrometry (SIMS), total reflection X-ray fluorescence spectrometry (TXRF) was applied to screen the sample for the presence of uranium particles. By the use of Si carriers in TXRF analysis, the detection limit of 22 pg was achieved for uranium. By combining these methods with SIMS, the isotope ratios of 235 U/ 238 U for individual uranium particles were efficiently determined. (author)

TXRF, PIXE and EDXRF: a first step towards normalization of x-ray spectrometry for chemical analysis

International Nuclear Information System (INIS)

Barreiros, M.A.; Costa, M.M.; Palha, M.; Pinheiro, T.; Araujo, M.F.; Silva, R.C. da

2000-01-01

Nowadays, many research studies rely on analytical measurements to which x-ray spectrometry techniques are particularly adequate. Because they are multi-elemental, versatile, fast and can reach low detection limits they are often applied to environmental and biomedical studies. Besides, they are able to provide reliable and accurate results. As also occurs with other analytical procedures, the quality assurance for non-routine analysis in R and D laboratories, is much less well established. when compared with routine analytical work. Thus, it is of foremost importance, to set the major quality parameters that significantly affect the quality of results. In addition, there is a need to apply the new concepts of trace ability and uncertainty to these techniques. This work reports on the reliability of TXRF, PIXE and EDXRF measurements by evaluating the uncertainty and trace ability for elemental analysis. The set of experimental and statistical procedures used to ensure the quality of results relative to the proposed objectives, as well as the methods applied to estimate the uncertainties will be presented and discussed. The sample preparation procedures, analytical calibration and spectral evaluation will be the parameters examined in this inter-laboratory study. The sample preparation procedures comprise pressure acid digestion and pelletizing for solid samples. The internal quality control for analytical calibration and spectral analysis is performed using certified reference materials and standard solutions. The goal of this work is to present a first step towards normalization of x-ray spectrometry techniques for chemical analysis. (author)

Comparison between energy dispersive X-ray fluorescence and other nuclear analytical techniques in mineral exploration and mining

International Nuclear Information System (INIS)

Clayton, C.G.; Packer, T.W.; Wormald, M.R.

1979-01-01

At the present time there is an increasing awareness of the value and need for in-situ analytical methods throughout the general area of mineral exploration and mining. Of the alternative techniques, the measurement of natural gamma radiation is well established for uranium exploration and it is now being developed for sea-bed and lake-bed surveying. Energy dispersive X-ray fluorescence equipment is becoming more generally accepted, especially for mine control. Neutron techniques, for so long used routinely in oil well logging, are now being developed for a wide range of applications in all aspects of exploration and mining. It is believed that these techniques will result in major applications in the future. The present paper compares the principal characteristics of energy dispersive X-ray fluorescence and neutron techniques in particular, with special emphasis being given to those factors which affect the accuracy of analytical content; such as elemental resolution, matrix effects, material heterogeneity and neutron transport. A generalised comparison between the techniques is difficult to achieve because of the different nature of radiation interactions, but a range of applications is described and these show the complementary nature of the methods and point to the areas for more active development in the future. (author)

Analysis of metal-laden water via portable X-ray fluorescence spectrometry

Science.gov (United States)

Pearson, Delaina; Weindorf, David C.; Chakraborty, Somsubhra; Li, Bin; Koch, Jaco; Van Deventer, Piet; de Wet, Jandre; Kusi, Nana Yaw

2018-06-01

A rapid method for in-situ elemental composition analysis of metal-laden water would be indispensable for studying polluted water. Current analytical lab methods to determine water quality include flame atomic absorption spectrometry (FAAS), atomic absorption spectrophotometry (AAS), electrothermal atomic absorption spectrometry (EAAS), and inductively coupled plasma (ICP) spectroscopy. However only two field methods, colorimetry and absorptiometry, exist for elemental analysis of water. Portable X-ray fluorescence (PXRF) spectrometry is an effective method for elemental analysis of soil, sediment, and other matrices. However, the accuracy of PXRF is known to be affected while scanning moisture-laden soil samples. This study sought to statistically establish PXRF's predictive ability for various elements in water at different concentrations relative to inductively coupled plasma atomic emission spectroscopy (ICP-AES). A total of 390 metal-laden water samples collected from leaching columns of mine tailings in South Africa were analyzed via PXRF and ICP-AES. The PXRF showed differential effectiveness in elemental quantification. For the collected water samples, the best relationships between ICP and PXRF elemental data were obtained for K and Cu (R2 = 0.92). However, when scanning ICP calibration solutions with elements in isolation, PXRF results indicated near perfect agreement; Ca, K, Fe, Cu and Pb produced an R2 of 0.99 while Zn and Mn produced an R2 of 1.00. The utilization of multiple PXRF (stacked) beams produced stronger correlation to ICP relative to the use of a single beam in isolation. The results of this study demonstrated the PXRF's ability to satisfactorily predict the composition of metal-laden water as reported by ICP for several elements. Additionally this study indicated the need for a "Water Mode" calibration for the PXRF and demonstrates the potential of PXRF for future study of polluted or contaminated waters.

Elemental characterization of alloy composition by wavelength dispersive X-ray fluorescence spectrometer

International Nuclear Information System (INIS)

Khan, F.A.; Pandey, A.; Das, D.K.; Behere, P.G; Mohd Afzal

2015-01-01

Wave length Dispersive X-ray Fluorescence (WD-XRF) is a non-destructive well-established analytical technique widely used in industrial and research applications for materials characterization. In nuclear industry various types of alloys have been used as per their application and importance. Few of them like SS-304, SS-316 and SS-316L are being regularly used for manufacturing of glove boxes at AFFF SS-304 alloy has been used in glove boxes of production line of MOX fuel due to its corrosive resistance and SS-316L is being used in chemical quality control lab and microwave applicator due to its acidic resistivity. In view of this an endeavor has been taken up to characterize these alloy steel. The experiments were carried out using a Rigaku make 'supermini', WD-XRF spectrometer having 200W Pd X-ray tube, 12 sample holder position, scintillation and proportional counters as a detector. All the parameters such as kV, mA, collimator, crystal and detectors were selected and operated via computer as per the given programme except for the sample preparation. EZscan (Energy Atomic Number Scan) technique is applied for the analysis of the above samples and the results obtained were in close agreement with the standard values. The present paper describes the characterization of SS-304L and SS-316L which have got better corrosion resistance properties against acids due to its compositions and suited for glove box manufacturing. (author)

Development of wave length-dispersive soft x-ray emission spectrometers for transmission electron microscopes - an introduction of valence electron spectroscopy for transmission electron microscopy

International Nuclear Information System (INIS)

Terauchi, Masami; Koike, Masato; Fukushima, Kurio; Kimura, Atsushi

2010-01-01

Two types of wavelength-dispersive soft X-ray spectrometers, a high-dispersion type and a conventional one, for transmission electron microscopes were constructed. Those spectrometers were used to study the electronic states of valence electrons (bonding electrons). Both spectrometers extended the acceptable energy regions to higher than 2000 eV. The best energy resolution of 0.08 eV was obtained for an Al L-emission spectrum by using the high-dispersion type spectrometer. By using the spectrometer, C K-emission of carbon allotropes, Cu L-emission of Cu 1-x Zn x alloys and Pt M-emission spectra were presented. The FWHM value of 12 eV was obtained for the Pt Mα-emission peak. The performance of the conventional one was also presented for ZnS and a section specimen of a multilayer device. W-M and Si-K emissions were clearly resolved. Soft X-ray emission spectroscopy based on transmission electron microscopy (TEM) has an advantage for obtaining spectra from a single crystalline specimen with a defined crystal setting. As an example of anisotropic soft X-ray emission, C K-emission spectra of single crystalline graphite with different crystal settings were presented. From the spectra, density of states of π- and σ-bondings were separately derived. These results demonstrated a method to analyse the electronic states of valence electrons of materials in the nanometre scale based on TEM. (author)

System for Gamma an X rays fluorescence spectrometric

International Nuclear Information System (INIS)

Alonso Abad, D.; Arista Romeu, E.; Bolanos Perez, L. and others

1997-01-01

A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

Energy dispersive X-ray fluorescence analysis of ancient coins: The case of Greek silver drachmae from the Emporion site in Spain

International Nuclear Information System (INIS)

Pitarch, A.; Queralt, I.

2010-01-01

Greek colonizers arrived at the Iberian Peninsula at the beginning of the sixth century B.C. and founded a small colony known as Emporion in north-east Spain. By the fifth century B.C., this colony became a small polis with a well-organized administrative structure. In this context, the necessity of coinage was a fact and the first coins were minted. Some of these coins were characterized by using energy dispersive X-ray fluorescence equipment. The analytical study focused on the elemental characterization of the coins minted from the fourth century to the first century B.C. and their compositional evolution during this period. The investigation has pointed out a very high fineness of the alloys throughout the time, with an average silver content around 98.32%, and the feasibility of energy dispersive X-ray fluorescence as a screening tool for the characterization of the alloys.

The design and fabrication of power splitter used in the timescale system of soft X-ray energy dispersive spectrometer in ICF experiment

International Nuclear Information System (INIS)

Zhang Huige; China Academy of Engineering Physics, Mianyang; Bai Lixin; Yu Ruizhen; Yang Cunbang; Su Cunxiao

2006-01-01

An improved eight power splitter is designed and fabricated newly, which is crucial in the time-scale system of soft X-ray energy dispersive spectrometer. The spectrometer is used in ICF laser facility to measure the evolution of soft X-ray spectrum, whose duration is only several nanoseconds. The synchronization and high bandwidth of signals produced by power splitter are tested, which shows the power splitter could meet the strict requirements of the experiments. The discussion of further improvement of power splitter are also presented. (authors)

Soft X-ray radiation damage in EM-CCDs used for Resonant Inelastic X-ray Scattering

Science.gov (United States)

Gopinath, D.; Soman, M.; Holland, A.; Keelan, J.; Hall, D.; Holland, K.; Colebrook, D.

2018-02-01

Advancement in synchrotron and free electron laser facilities means that X-ray beams with higher intensity than ever before are being created. The high brilliance of the X-ray beam, as well as the ability to use a range of X-ray energies, means that they can be used in a wide range of applications. One such application is Resonant Inelastic X-ray Scattering (RIXS). RIXS uses the intense and tuneable X-ray beams in order to investigate the electronic structure of materials. The photons are focused onto a sample material and the scattered X-ray beam is diffracted off a high resolution grating to disperse the X-ray energies onto a position sensitive detector. Whilst several factors affect the total system energy resolution, the performance of RIXS experiments can be limited by the spatial resolution of the detector used. Electron-Multiplying CCDs (EM-CCDs) at high gain in combination with centroiding of the photon charge cloud across several detector pixels can lead to sub-pixel spatial resolution of 2-3 μm. X-ray radiation can cause damage to CCDs through ionisation damage resulting in increases in dark current and/or a shift in flat band voltage. Understanding the effect of radiation damage on EM-CCDs is important in order to predict lifetime as well as the change in performance over time. Two CCD-97s were taken to PTB at BESSY II and irradiated with large doses of soft X-rays in order to probe the front and back surfaces of the device. The dark current was shown to decay over time with two different exponential components to it. This paper will discuss the use of EM-CCDs for readout of RIXS spectrometers, and limitations on spatial resolution, together with any limitations on instrument use which may arise from X-ray-induced radiation damage.

Preliminary results on air pollution inside an iron metallurgical plant, using rotating streaker sampler and energy dispersive X-ray microfluorescence

International Nuclear Information System (INIS)

Nascimento Filho, V.F.; Silva, R.M.C.; Perez, C.A.

2005-01-01

Our aim was to study the chemical concentration of some metals in suspended particulate matter inside an-iron metallurgical plant. Using a rotating streaker air-particulate sampler with 8 and 0.45 microns pore diameter filter, it was possible to collect coarse and fine particulates during a week, with one hour step. After this, each strip of the filter was analyzed by energy dispersive x-ray microfluorescence (μ-EDXRF), using in the excitation a collimated x-ray line beam from a Mo target tube (30 kV, 20 mA, Zr filter) with a quartz capillary (120 mm long, 10 mm entrance diameter and 20 microns inner diameter at exit). The detection was carried out using a Si(Li) semiconductor detector coupled to a multichannel analyzer, and the X-ray spectra were fitted with the AXIL software. The profiles of several elements are shown and the results are discussed.

Threat detection of liquid explosives and precursors from their x-ray scattering pattern using energy dispersive detector technology

DEFF Research Database (Denmark)

Kehres, Jan; Olsen, Ulrik Lund; Lyksborg, Mark

2017-01-01

Energy dispersive X-ray diffraction (EDXRD) can be applied for identification of liquid threats in luggage scanning in security applications. To define the instrumental design, the framework for data reduction and analysis and test the performance of the threat detection in various scenarios....... Initial testing of the threat detection algorithms with this data set indicate the feasibility of detection levels of > 95 % true positive with

European X-ray spectroscopy and polarimetry payload for Spacelab

Energy Technology Data Exchange (ETDEWEB)

Andresen, R D; Whitcomb, G [European Space Research and Technology Centre, Noordwijk (Netherlands); Brinkman, A C [Space Research Laboratory, Utrecht, The Netherlands; Beuermann, K [Max-Planck-Institut fuer Physik und Astrophysik, Garching/Muenchen (Germany, F.R.). Inst. fuer Extraterrestrische Physik; Culhane, J L [University Coll., London (UK). Mullard Space Science Lab.; Griffiths, R [Leicester Univ. (UK); Manno, V [ESA Headquarters, Paris, France; Rocchia, R [CEA Centre d' Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France)

1976-08-01

A group of instruments for X-ray spectroscopy and polarimetry studies of a number of cosmic X-ray sources is being designed for possible use on Spacelab. Large area Bragg spectrometers and polarimeters for photon energies above 2 keV are described. For the energy range below 2 keV, both dispersive and non-dispersive spectrometers are employed at the common focus of a nested array of paraboloids. Following a brief outline of the scientific background to the mission, the properties of the individual instruments are discussed.

The study of electric erosion treatments of Ni-superalloys by ion-scattering spectrometry and X-ray analysis

International Nuclear Information System (INIS)

Betsofen, S.Ya.; Borisov, A.M.; Sarychev, S.M.; Romanovskij, E.A.; Bakui Ali; Bespalova, O.V.; Kulikauskas, V.S.; Serkov, M.V.; Grigorovich, K.V.

2004-01-01

The study results are reported for a surface layer of a nickel base heat resistant alloy of the following composition, mas.%: Ni-8.2 Cr-10.5 W-15.5 Co-2.4 Mo-1.4 Nb-4.8 Al-0.2 C, after electroerosion. With the use of Rutherford and nuclear backscattering spectrometry and X-ray diffraction analysis it is revealed that melting under electroerosion results in redistribution of alloying elements, enrichment with carbon and occurrence of residual tensile stresses [ru

Illicit drug detection using energy dispersive x-ray diffraction

Science.gov (United States)

Cook, E. J.; Griffiths, J. A.; Koutalonis, M.; Gent, C.; Pani, S.; Horrocks, J. A.; George, L.; Hardwick, S.; Speller, R.

2009-05-01

Illicit drugs are imported into countries in myriad ways, including via the postal system and courier services. An automated system is required to detect drugs in parcels for which X-ray diffraction is a suitable technique as it is non-destructive, material specific and uses X-rays of sufficiently high energy to penetrate parcels containing a range of attenuating materials. A database has been constructed containing the measured powder diffraction profiles of several thousand materials likely to be found in parcels. These include drugs, cutting agents, packaging and other innocuous materials. A software model has been developed using these data to predict the diffraction profiles which would be obtained by X-ray diffraction systems with a range of suggested detector (high purity germanium, CZT and scintillation), source and collimation options. The aim of the model was to identify the most promising system geometries, which was done with the aid of multivariate analysis (MVA). The most promising systems were constructed and tested. The diffraction profiles of a range of materials have been measured and used to both validate the model and to identify the presence of drugs in sample packages.

Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens.

Science.gov (United States)

Lu, Ping; Yuan, Renliang; Zuo, Jian Min

2017-02-01

Elemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm2 with the acquisition time of ~2 s or less. Here we report the details of this method, and, in particular, investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO3 in [001] projection for 200 keV electrons.

Heavy metal determination by X-rays spectrometry for superficial sediments at Guantanamo bay

International Nuclear Information System (INIS)

Gelen, A.; Izquierdo; Corrales, W. Y.; Lopez, N.; Casanova, A. O.; Diaz, O.; Manso, M.V.; D Alessandro, K.; Reyes, E.; Toledo, C.; Ruiz, F.; Ramirez, M.; Beltran, J.; Martin, A.

2007-01-01

Twelve surface samples of the Guantanamo Bay (Cuba) were collected and analysed by X-Rays Spectrometry. Twenty one elements (Si, Ca, K, Na, P, S, Cl, Al, Fe, Mg, Ti, Mn, C, O, Cr, Cu, Ni, Co, Pb, V and Zn) have been determined. The distribution of the metals is associated with the wastewater from anthropogenic origin that receives the bay, mainly by fluvial currents. Multivariate statistical were used for the analysis of the results. Finally the results analysed were compared with the analysis performed by Engineering Centre for Environmental Management of Bays and Coasts (Cimab) using Inductively Coupled Plasma Emission (ICP) for some elements such as: Cr, Cu, Fe, Ni, Pb, V and Zn. The results show the Guantanamo Bay is less polluted than others Cuban Bays. (Author)

Heavy ion recoil spectrometry of SixGe1-x thin films

International Nuclear Information System (INIS)

Walker, S.R.; Johnston, P.N.; Bubb, I.F.; Cohen, D.D.; Dytlewski, N.; Hult, M.; Whitlow, H.J.; Zaring, C.; Oestling, M.

1993-01-01

Mass and energy dispersive recoil spectrometry employing 77 MeV 127 I ions from ANTARES (FN Tandem) facility at Lucas Heights has been used to examine the isotopic composition of samples of Si x Ge 1-x grown at the Australian National University by Electron Beam Evaporation (EBE). The recoiling target nuclei were analysed by a Time Of Flight and Energy (TOF-E) detector telescope composed of two timing pickoff detectors and a surface barrier (energy) detector. From the time of flight and energy, the ion mass can be determined and individual depth distributions for each element can be obtained. Recoil spectrometry has shown the presence of oxygen in the Si x Ge 1-x layer and has enabled the separate determination of energy spectra for individual elements. 9 refs., 3 figs

Ship-Borne Geochemical Investigations of Deep-Sea Manganese-Nodule Deposits in the Pacific Using a Radioisotope Energy-Dispersive X-Ray System

DEFF Research Database (Denmark)

Friedrich, G.H.W.; Kunzendorf, Helmar; Plüger, W.L.

1974-01-01

A radioisotope energy-dispersive X-ray (EDX) system has been used on board the German research vessel “Valdivia” during an exploration expedition in the northern equatorial Pacific in 1973. The instrumentation used consisted of an X-ray detection system incorporating a 30 mm2 effective-area Si (Li......) detector with a measured energy resolution of 195 eV for Mn Kα X-rays, standard nuclear electronics, a 1024-channel analyser and a data read-out unit. The X-ray spectra in the manganese-nodule samples were excited by a 30-mCi 238Pu source. The six elements Mn, Fe, Co, Ni, Cu and Zn were analysed on board....... Precision values for the analyses were less than 3% for Mn, Fe, Ni, Cu and Zn and about 5% for Co. A total amount of 350 analyses was carried out during a one-month cruise. Average contents of 190 analysed whole manganese-nodule samples from all the sampling sites of the covered area were 23.3% Mn, 6.7% Fe...

MOS solid-state detector arrays for x-ray imaging

International Nuclear Information System (INIS)

Koppel, L.N.

1977-01-01

Two types of MOS detector arrays were used to sense directly patterns of soft x-rays, in the Lawrence Livermore Laboratory experimental laser-fusion program. A linear self-scanning photodiode array (SSPA) is used in a wave-length-dispersive spectrometer. A frame transfer charge-coupled device (CCD) facilitates the use of an x-ray microscope. Measurements and calculations of the x-ray sensitivity of these devices are presented. Their linearity and dynamic range are discussed, as well as data recovery systems for each detector. Experiences in using these devices to detect pulses of x-rays in laser-fusion experiments are described

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

Science.gov (United States)

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

2012-01-01

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

Thermoelectrically cooled semiconductor detectors for non-destructive analysis of works of art by means of energy dispersive X-ray fluorescence

CERN Document Server

Cesareo, R; Castellano, A

1999-01-01

Thermoelectrically cooled semiconductor detectors, such as Si-PIN, Si-drift, Cd sub 1 sub - sub x Zn sub x Te and HgI sub 2 , coupled to miniaturized low-power X-ray tubes, are well suited in portable systems for energy-dispersive X-ray fluorescence (EDXRF), analysis of archaeological samples. The Si-PIN detector is characterized by a thickness of about 300 mu m, an area of about 2x3 mm sup 2 , an energy resolution of about 200-250 eV at 5.9 keV and an entrance window of 25-75 mu m. The Si-drift detector has approximately the same area and thickness, but an energy resolution of 155 eV at 5.9 keV. The efficiency of these detectors is around 100% from 4 to 10 keV, and then decreases versus energy, reaching approx 9% at 30 keV. Coupled to a miniaturized 10 kV, 0.1 mA, Ca-anode or to a miniaturized 30 kV, 0.1 mA, W-anode X-ray tubes, portable systems can be constructed, which are able to analyse K-lines of elements up to about silver, and L-lines of heavy elements. The Cd sub 1 sub - sub x Zn sub x Te detector ha...

Feasibility of wavelength dispersive X-ray fluorescence spectrometry for a simplified analysis of bromine in water samples with the aid of a strong anion exchange disk

International Nuclear Information System (INIS)

An, Jinsung; Jung, Hyeyeon; Bae, Jo-Ri; Yoon, Hye-On; Seo, Jungju

2014-01-01

The feasibility of wavelength dispersive X-ray fluorescence spectrometry (WDXRF) for a simplified analysis of bromine (Br) in water samples with the aid of strong anion exchange (SAX) disk was assessed in this study. Dissolved Br in the water sample was pre-concentrated on the SAX disk and directly analyzed by WDXRF without an elution step. The SAX disk was capable of fully adsorbing both bromide (Br − ) and bromate (BrO 3 − ) on its surface owing to their anionic properties, regardless of the pH level of environmental samples. The SAX–WDXRF system was examined using calibration standards (i.e., SAX disks with specific amounts of Br retained; 1, 10, 50, 100 and 500 μg), and a determination coefficient of R 2 = 0.9999 was yielded. The system had a low detection limit for Br (limit of detection = 0.253 μg for Br on the SAX disk) with good reproducibility (relative standard error (RSE) = 4–7%). Spike and inter-comparison tests were performed to confirm the accuracy of the proposed SAX–WDXRF method. Both tests exhibited reasonable accuracy (RSE = 3–6%). The method is simple and easy, indicating a great possibility of application in various environmental sample types, especially for which a simplified analytical system for the determination of Br is urgently required. - Highlights: • Bromide and bromate were entirely retained on a strong anion exchange (SAX) disk. • The SAX disk was used to pre-concentrate dissolved Br species from water samples. • The SAX disk adsorbing dissolved Br was directly analyzed by WDXRF. • The accuracy of the SAX–WDXRF method was confirmed by spike and inter-comparison tests. • Rapid and sensitive Br analysis can be achieved using the proposed SAX–WDXRF method

Pre-Columbian alloys from the royal tombs of Sipan; energy dispersive X-ray fluorescence analysis with a portable equipment

International Nuclear Information System (INIS)

Cesareo, R.; Calza, C.; Dos Anjos, M.; Lopes, R.T.; Bustamante, A.; Fabian S, J.; Alva, W.; Chero Z, L.

2010-01-01

On the north coast of present-day Peru flourished approximately between 50 and 700 AD, the Moche civilization. It was an advanced culture and the Moche were sophisticated metalsmiths, so that they are considered as the finest producers of jewels and artefacts of the region. The Moche metalworking ability was impressively demonstrated by the objects discovered by Walter Alva and coworkers in 1987, in the excavations of the 'Tumbas Reales de Sipan'. About 50 metal objects from these excavations, now at the namesake Museum, in Lambayeque, north of Peru, were analyzed with a portable equipment using energy-dispersive X-ray fluorescence. This portable equipment is mainly composed of a small size X-ray tube and a thermoelectrically cooled X-ray detector. Standard samples of gold and silver alloys were employed for quantitative analysis. It was determined that the analyzed artefacts from the 'Tumbas Reales de Sipan' are mainly composed of gold, silver and copper alloys, of gilded copper and of tumbaga, the last being a poor gold alloy enriched at the surface by depletion gilding, i.e. removing copper from the surface.

Energy-dispersive X-ray fluorescence of discarded tire samples, using a Si-PIN detector

International Nuclear Information System (INIS)

Lopes, Fabio; Appoloni, C.R.; Melquiades, Fabio L.

2007-01-01

The determination of zinc concentration in samples of discarded tires is of great environmental interest because the process for manufacturing tyres uses S for rubber vulcanization, and ZnO is the reaction catalyst. Discarded tyres are being used in asphalt paving, in the burning process of thermoelectric and cement industries and also for controlling erosion in agricultural areas. Analysis of tyre samples usually requires chemical digestion which is slow and expensive. Aiming to eliminate those limitations, this work uses energy-dispersive X-ray fluorescence (EDXRF) with a portable equipment, once it is a simultaneous multi-element analytical technique, requiring minimal sample preparation. Five samples of discarded tyres have been ground and analysed in the form of pastilles, using a mini X-ray tube (Ag target, MO filter, 25 kV/20 μA) for 200 s, and a Si-PIN semiconductor detector coupled to a multichannel analyser. Zinc concentrations in the range of 40.6 to 44.2 μg g -1 have been obtained, representing 0.4% of the tire composition, which is below the maximum value (2%) recommended by the European Tyre Recycling Association. Concentrations between 0.15 and 0.52 μg g -1 were obtained for Fe

Fast GPU-based spot extraction for energy-dispersive X-ray Laue diffraction

International Nuclear Information System (INIS)

Alghabi, F.; Schipper, U.; Kolb, A.; Send, S.; Abboud, A.; Pashniak, N.; Pietsch, U.

2014-01-01

This paper describes a novel method for fast online analysis of X-ray Laue spots taken by means of an energy-dispersive X-ray 2D detector. Current pnCCD detectors typically operate at some 100 Hz (up to a maximum of 400 Hz) and have a resolution of 384 × 384 pixels, future devices head for even higher pixel counts and frame rates. The proposed online data analysis is based on a computer utilizing multiple Graphics Processing Units (GPUs), which allow for fast and parallel data processing. Our multi-GPU based algorithm is compliant with the rules of stream-based data processing, for which GPUs are optimized. The paper's main contribution is therefore an alternative algorithm for the determination of spot positions and energies over the full sequence of pnCCD data frames. Furthermore, an improved background suppression algorithm is presented.The resulting system is able to process data at the maximum acquisition rate of 400 Hz. We present a detailed analysis of the spot positions and energies deduced from a prior (single-core) CPU-based and the novel GPU-based data processing, showing that the parallel computed results using the GPU implementation are at least of the same quality as prior CPU-based results. Furthermore, the GPU-based algorithm is able to speed up the data processing by a factor of 7 (in comparison to single-core CPU-based algorithm) which effectively makes the detector system more suitable for online data processing

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

Energy Technology Data Exchange (ETDEWEB)

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

2004-10-08

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

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

International Nuclear Information System (INIS)

Echard, Jean-Philippe

2004-01-01

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

Energy dispersive soft X-ray fluorescence analysis by radioisotopic α-particle excitation

International Nuclear Information System (INIS)

Robertson, R.

1977-01-01

A Si(Li) X-ray detector system and 210 Po α-particle excitation source are combined to form a spectrometer for low energy X-rays. Its response in terms of Ksub(α) X-ray rate is shown for thick targets of elements from fluorine to copper. Potential applications of the equipment to useful quantitative elemental analysis of geological, biological and organic materials are explored. The results of analyses for oxygen and silicon in rocks and potassium in vegetation samples are included. A semi-empirical method of correcting for absorption and enhancement effects is employed. This is based upon X-ray production and photon absorption cross-sections taken from the literature and upon a minimal number of experimentally derived coefficients. (Auth.)

Determination of sulphur with total reflection x-ray spectrometry

International Nuclear Information System (INIS)

Steinmeyer, S.; Kolbesen, B.O.

2000-01-01

The potential and limitations of total reflection x-ray spectrometry (TXRF) were tested for the quantitative determination of the light element sulphur in inorganic and biological samples. As representatives of inorganic samples alkali, transition metal, magnesium and aluminum sulphates were investigated. As biological samples the sulphur containing amino acid methionine and the pharmaceutical drug insulin were chosen. All measurements were performed on a TXRF-spectrometer EXTRA IIA (Atomika Instruments, Oberschleissheim/Germany) using tungsten L-radiation as the excitation tube. Various concentrations of all samples ranging from 20 mg/l to 0.5 mg/l were determined. In addition the surface topography and thickness of the dry residue of these samples were investigated with SEM and a thickness profilometer (Alpha-Step). The result show that the reliable determination of sulphur in sulphates depends on the cation involved. Alkali sulphates like Na 2 SO 4 , or K 2 SO 4 form bulky residues resulting in significant deviations of the recovery rate of sulphur. In this case the use of smoothing detergents like 1 % HF, 1 % malic acid and 2 % hydrazinhydrat was found to be necessary for accurate determination. The results for the biological samples agree well with the expected values. The investigations lead to the conclusion that TXRF combined with a proper samples preparation is well suited for the determination of sulphur in different samples with various concentrations and matrices. (author)

Determination of Fe in blood using portable X-ray fluorescence spectrometry: an alternative for sports medicine

International Nuclear Information System (INIS)

Zamboni, C.B.; Metairon, S.; Kovacs, L.; Macedo, D.V.; Rizzutto, M.A.

2016-01-01

An alternate methodology based on a portable X-ray fluorescence spectrometry (PXRFS) for determination of Fe in blood was evaluated. The iron concentrations was determined in whole blood of 18 male amateur athletes (runners) using this portable XRF spectrometer and compared with a control group (54 male donors at the same age but not involved with physical activities) obtained by XRF and NAA techniques. The Fe concentration in the blood of runners is an important factor in sports medicine contributing to the performance of endurance athletes as well as for proposing new protocols of clinical evaluation. (author)

Calibration comparative results for X - and gamma ray spectrometry with HPGe and BEGe detectors for a radon reference chamber

International Nuclear Information System (INIS)

Zoran, Maria; Paul, Annette; Arnold, Dirk

2002-01-01

Inhaled decay products of 222 Rn are the dominant components of the natural radiation exposure being responsible for about 30% of the whole human radioactive exposure. Field instruments for 222 Rn and his progeny monitoring are calibrated in 'radon climate rooms', where it is possible to vary and monitor 222 Rn and the indoor air parameters ( temperature, humidity, ventilation rate, aerosol concentration). German radon reference chamber used was developed and installed at the Physikalisch-Technische Bundesanstalt in order to serve as a metrological standard for radon and his progeny calibration of active and passive, indoor and outdoor radon monitoring devices in air climate. The basic parts of experimental setup for this γ and X -ray spectrometry analysis consists of a γ-X ray source in a lead shield/collimator, the detectors, the electronics necessary for pulse-height analysis (PHA) to obtain energy spectra. For calibrating system with 226 Ra standard sources (multienergy X ray and gamma emitters), two germanium detectors HPGe (12.5 nominal efficiency) and BEGe (22.5 nominal efficiency) were used. Germanium detectors are semiconductor diodes having a P-I-N structure in which the Intrinsic (I) region is sensitive to ionizing radiation, particularly X-rays and gamma rays. The BEGe is designed with an electrode structure that enhances low energy resolution and is fabricated from selected germanium having an impurity profile that improves charge collection (thus resolution and peak shape) at high energies which is really important in analysis of the complex spectra for uranium and finally for 226 Ra. MAESTRO MCA software and GNUPLOT program were used for spectra acquisition and spectra analysis, respectively . The main aim of this paper was to do a comparatively analysis of the detector performances for this radon chamber spectrometric chain. The calibration data analysis includes energy calibrations for both detection systems as well as comparative X and gamma

Determination of trace metals in nuclear-grade uranium dioxide by X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Salvador, V.L.R.; Imakuma, K.

1988-04-01

A method is described for the simultaneous determination of low concentrations of Ca, Cr, Cu, Fe, Mn and Ni in nuclear-grade uranium dioxide by X-ray fluorescence spectrometry, without the use of chemical treatment. The lower limits of detection range from 2 μg g -1 for nickel and manganese to 5 μg g -1 for copper. Samples are prepared in the form of double-layer pellets with boric acid as a binding agent. Standards are prepared in a U 3 O 8 matrix, which is more chemically stable than UO 2 and has similar matrix behaviour. The correlation coefficients for calibration curves are better than 0.999. Erros range from 2.4 % for chromium to 6.8 % for nickel. (author) [pt

Cefuroxime axetil solid dispersions prepared using solution enhanced dispersion by supercritical fluids.

Science.gov (United States)

Jun, Seoung Wook; Kim, Min-Soo; Jo, Guk Hyun; Lee, Sibeum; Woo, Jong Soo; Park, Jeong-Sook; Hwang, Sung-Joo

2005-12-01

Cefuroxime axetil (CA) solid dispersions with HPMC 2910/PVP K-30 were prepared using solution enhanced dispersion by supercritical fluids (SEDS) in an effort to increase the dissolution rate of poorly water-soluble drugs. Their physicochemical properties in solid state were characterized by differential scanning calorimeter (DSC), powder X-ray diffraction (PXRD), Fourier transform infrared spectrometry (FT-IR) and scanning electron microscopy. No endothermic and characteristic diffraction peaks corresponding to CA were observed for the solid dispersions in DSC and PXRD. FTIR analysis demonstrated the presence of intermolecular hydrogen bonds between CA and HPMC 2910/PVP K-30 in solid dispersions, resulting in the formation of amorphous or non-crystalline CA. Dissolution studies indicated that the dissolution rates were remarkably increased in solid dispersions compared with those in the physical mixture and drug alone. In conclusion, an amorphous or non-crystalline CA solid dispersion prepared using SEDS could be very useful for the formulation of solid dosage forms.

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

Science.gov (United States)

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.

X-ray microscopy and spectromicroscopy - tools for environmental studies

International Nuclear Information System (INIS)

Thieme, J.

2002-01-01

microscopy, especially structures from soils, sediments and groundwater aquifers. Several examples will be presented: Dispersions extracted from these systems have been imaged with an X-ray microscope to obtain first of all a visual impression of the appearance of the colloids. The effect of changing chemical conditions in the aqueous dispersion media has been studied, too. The change in the appearance of the colloidal structures has been imaged and evaluated using fractal geometry. Clay dispersions and microhabitats have been imaged tomographically. Tilt series of images have been obtained with an X-ray microscope; the specimen was then reconstructed from these images. The resulting reconstruction conveys a detailed three-dimensional impression of the specimen structure, as will be shown. Using spectromicroscopy, the distribution of organic substances on inorganic soil colloids has been studied. A major fraction of these are humic substances. Spectra have been taken from humic substances with and without iron as a coagulation agent. Different functional groups have been identified and changes due to the influence of iron have been mapped. Copyright (2002) Australian Society for Electron Microscopy Inc

X-ray fluorescence spectrometry analysis of soil heavy metals in a populous place and evaluation on its heavy metals pollution

International Nuclear Information System (INIS)

Li Dan; Wang Guangxi; Luo Yaoyao; Qiu Luyang

2012-01-01

Abstract The contents of As, Cr, Pb, Cu, Zn and Ni in soil of the populous place, were determined by X-ray fluorescence spectrometry. The heavy metals pollution of soil was evaluated by using single pollute index, synthesis pollute index, geoaccumulation index and potential ecological risk index, and the results showed that the populous place was in the state of slight pollution and ecological risk. (authors)

Dispersive X-ray fluorescence applications in energy in environmental problems diagnostic

International Nuclear Information System (INIS)

Odino, R.; Souto, B.; Roca, S.; Campomar, W.

1994-01-01

X-ray fluorescence energy was used to detect the grade of contamination due to a Portland cement factory. X-ray fluorescence was used to determine the incidence of a Portland cement plant in the quality of air in its surroundings. Many contaminants (Cu, Pb, Ni, Br) do not come from the Portland cement industry but other industries in the zone

A manual to the MAXRAY program library for reflective and dispersive ray tracing

International Nuclear Information System (INIS)

Svensson, S.; Nyholm, R.

1985-07-01

A general ray tracing program package for reflective and dispersive X-ray optics is described. The package consists of a number of subroutines written in FORTRAN 77 code giving the necessary tools for ray tracing. The program package is available on request from the authors. (authors)

Relative evaluation of neutron activation, X-ray fluorescence and spark source mass spectrometry for multielement analysis of geothermal waters

International Nuclear Information System (INIS)

Blommaert, W.; Vandelannoote, R.; Van't Dack, L.; Gijbels, R.; Van Grieken, R.

1980-01-01

To sulfide geothermal waters from the French Pyrenees region and bicarbonate and chloride waters from the French Vosges area, all of the following analysis techniques were applied in order to compose a broad inventory of trace elements: (1) for the dissolved metarial: neutron activation analysis after a freeze-drying step using a very short cycle, short cycle or long cycle, neutron activation after co-crystallization on 1-(2-pyridylazo)-2-naphthol (PAN) using a short cycle or long cycle, X-ray fluorescence after co-crystallization on PAN and spark source mass spectrometry after evaporation on graphite or preconcentration on PAN, and, (2) for the filtered or suspended material: neutron activation using a very short, short or long cycle and X-ray fluorescence. Altogether, on the average some 30 elements could be determined above the detection limit in solution and 15 in suspension. (author)

Automatic Sample Changer for X-Ray Spectrometry

International Nuclear Information System (INIS)

Morales Tarre, Orlando; Diaz Castro, Maikel; Rivero Ramirez, Doris; Lopez Pino, Neivy

2011-01-01

The design and construction of an automatic sample changer for Nuclear Analysis Laboratory's X-ray spectrometer at InSTEC is presented by giving basic details about its mechanical structure, control circuits and the software application developed to interact with the data acquisition software of the multichannel analyzer. Results of some test experiments performed with the automatic sample changer are also discussed. The system is currently in use at InSTEC. (Author)

An attempt to reduce radioactivity for energy-dispersive x-ray analysis

International Nuclear Information System (INIS)

Hamada, S.

1992-01-01

The object of this work is to develop a specimen preparation technique which reduces the intensity of radioactivity of a neutron-irradiated materials for microchemical analysis by analytical electron microscope (AEM) with energy dispersive X-ray spectroscopy (EDXS). A composite specimen preparation technique for the AEM was developed using unirradiated materials. The technique reduced the mass of material from a dummy irradiated specimen by more than a factor of 100. A 1-mm diam. disk was punched from a dummy irradiated 3-mm diam. transmission electron microscope (TEM) disk. The 1-mm disk was then pressed into a hole previously punched at the center of a second 3 mm diam. disk creating a composite disk. The composite disk was electropolished using a twin jet Tenupol until the thickness of the center of the composite was about 100 μm. Approximately 100 μm of nickel plating was then deposited on the surface of the thinned composite. Standard electropolishing by Tenupol unit was performed on the nickel-plated composite specimen and the composite specimen was examined by TEM

Low energy x-ray spectrometer

International Nuclear Information System (INIS)

Woodruff, W.R.

1981-01-01

A subkilovolt spectrometer has been produced to permit high-energy-resolution, time-dependent x-ray intensity measurements. The diffracting element is a curved mica (d = 9.95A) crystal. To preclude higher order (n > 1) diffractions, a carbon x-ray mirror that reflects only photons with energies less than approx. 1.1 keV is utilized ahead of the diffracting element. The nominal energy range of interest is 800 to 900 eV. The diffracted photons are detected by a gold-surface photoelectric diode designed to have a very good frequency response, and whose current is recorded on an oscilloscope. A thin, aluminium light barrier is placed between the diffracting crystal and the photoelectric diode detector to keep any uv generated on or scattered by the crystal from illuminating the detector. High spectral energy resolution is provided by many photocathodes between 8- and 50-eV wide placed serially along the diffracted x-ray beam at the detector position. The spectrometer was calibrated for energy and energy dispersion using the Ni Lα 1 2 lines produced in the LLNL IONAC accelerator and in third order using a molybdenum target x-ray tube. For the latter calibration the carbon mirror was replaced by one surfaced with rhodium to raise the cut-off energy to about 3 keV. The carbon mirror reflection dependence on energy was measured using one of our Henke x-ray sources. The curved mica crystal diffraction efficiency was measured on our Low-Energy x-ray (LEX) machine. The spectrometer performs well although some changes in the way the x-ray mirror is held are desirable. 16 figures

X-ray studies, spectral characterization and thermal behaviour of a ...

African Journals Online (AJOL)

HP04)3]. H20, I, was synthesized by reacting Zn2+ ions with tris-(2-aminoethyl) amine phosphate [C6H21N4][P04].5H20. The compound was characterized by powder x-ray diffraction analysis, energy dispersive analysis by x-ray and infrared ...

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

Science.gov (United States)

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.

Handbook on Mobile Gamma-ray Spectrometry

DEFF Research Database (Denmark)

Aage, Helle Karina; Korsbech, Uffe C C

2003-01-01

Basic physics and mathematics for Airborne and Car-borne Gamma-ray Spectrometry supplemented with practical examples and methods for advanced data processing......Basic physics and mathematics for Airborne and Car-borne Gamma-ray Spectrometry supplemented with practical examples and methods for advanced data processing...

Trace rare earth analysis by neutron activation and γ-ray/x-ray spectrometry

International Nuclear Information System (INIS)

Laul, J.C.; Nielson, K.K.; Wogman, N.A.

1977-01-01

A rare earth group separation scheme followed by photon energy analysis using Ge(Li) and intrinsic Ge detectors enhances significantly the detection of individual rare earth elements (REE) at or below the ppb level. Based on the x-ray and selected γ-ray energies, Ge(Li) γ-ray counting is favorable for 140 La, 141 Ce, 142 Pr, 153 Sm, 171 Er, and 177 Lu, whereas intrinsic Ge γ-ray counting is favorable for 143 Ce, 147 Nd, 160 Tb, and 166 Ho, and intrinsic Ge x-ray counting is favorable for 152 Eu and 175 Yb. Gamma-ray counting of 153 Gd and 170 Tm is equally sensitive with Ge(Li) or intrinsic Ge detectors. Precise measurements of the REE were made in the USGS geological samples BCR-1, W-1, AGV-1, G2, GSP-1 and PCC-1, the IAEA Soil-5, and the NBS orchard leaf and bovine liver standards. Their chondritic normalized REE patterns behave as a smooth function of the REE ionic radii. Interestingly, the REE patterns observed in orchard leaf and other plants are identical to the REE pattern in bovine liver. This comparison leads us to suggest that the plant REE patterns are probably not further fractionated by animals such as bovine during their dietary plant uptake

X-ray cluster Abell 744

International Nuclear Information System (INIS)

Kurtz, M.J.; Huchra, J.P.; Beers, T.C.; Geller, M.J.; Gioia, I.M.

1985-01-01

X-ray and optical observations of the cluster of galaxies Abell 744 are presented. The X-ray flux (assuming H(0) = 100 km/s per Mpc) is about 9 x 10 to the 42nd erg/s. The X-ray source is extended, but shows no other structure. Photographic photometry (in Kron-Cousins R), calibrated by deep CCD frames, is presented for all galaxies brighter than 19th magnitude within 0.75 Mpc of the cluster center. The luminosity function is normal, and the isopleths show little evidence of substructure near the cluster center. The cluster has a dominant central galaxy, which is classified as a normal brightest-cluster elliptical on the basis of its luminosity profile. New redshifts were obtained for 26 galaxies in the vicinity of the cluster center; 20 appear to be cluster members. The spatial distribution of redshifts is peculiar; the dispersion within the 150 kpc core radius is much greater than outside. Abell 744 is similar to the nearby cluster Abell 1060. 31 references

Total reflection X-ray fluorescence and energy-dispersive X-ray ...

Indian Academy of Sciences (India)

(ICP-AES), atomic absorption spectrometry (AAS) and spark source mass spectrome- ... actinide oxides, for trace element determinations normal XRF cannot ... at a flat polished sample support at an angle less than the critical angle and thus ...

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

Science.gov (United States)

Echard, Jean-Philippe

2004-10-01

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

Spectrometry of X-ray beams using Cadmium and Zinc Teluride detector

International Nuclear Information System (INIS)

Becker, Paulo Henriques Bastos

1997-06-01

Determination of X-ray spectra to be utilized for medical diagnostics is a complementary process to the development of procedures to be applied to the quality control of radiodiagnostics X-ray equipment. Until some years ago, that was only possible using Germanium or Silicon detectors. Both have an excellent resolution in this energy range, but present also some restrictions as there are high costs and the necessity of operating them at temperature of liquid Nitrogen, which is not always available at the measurement's place. Room temperature detectors like Cadmium Telluride and Mercury Iodine don't have these restrictions. They, however, have a lower resolution and incomplete collection of the charges produced by their interaction with radiation. With technological advance of crystal growth in general and new techniques like cooling the crystal with a Peltier cell and rise time discrimination circuits, today Cadmium Telluride detectors show a resolution very close to that from Germanium detectors. This work relates to the routine use of Cadmium and Zinc Telluride detectors for measuring X-ray spectra in loco of diagnostic X-ray units. It characterizes the properties of a commercially available detector and offers a model for stripping the measured pulse height distribution. It was also developed a collimator to allow the direct measurement of the beam. The model developed and the constructed set-up were applied to two X-ray tubes and the achieved spectra compared with some spectra available from the literature. (author)

Caracterização dos níveis de elementos químicos em solo, submetido a diferentes sistemas de uso e manejo, utilizando espectrometria de fluorescência de raios-x por energia dispersiva (EDXRF Characterization of chemical elements in soil submitted to different systems use and management by energy dispersive x-ray fluorescence spectrometry (EDXRF

Directory of Open Access Journals (Sweden)

Arci Dirceu Wastowski

2010-01-01

Full Text Available This study aimed to evaluate the chemical elements levels in soil, submitted to different management systems and use by the Energy Dispersive X-Ray Fluorescence Spectrometry - EDXRF. The systems were T1 - agro forestry (SAF, T2 - Native Field (CN, T3 - Native Forest (NM, T4 - Tillage Forest (PF; T5 - conventional tillage system (SPC and T6 - System tillage (NT. Samples were collected at 0-10 and 10-20 cm, dried and ground for analysis in EDX-720. The soil showed no difference in the average concentrations of chemical elements analyzed in the profiles, but the systems presented different concentrations of metal elements, and T3 had the highest K, Ca and Zn at 0-10 cm and higher contents of K, Ca, Cu, Zn and Mn in the layer of 10-20 cm.

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

Science.gov (United States)

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.

Energy dispersive X-ray spectrometry study of the protective effects of fluoride varnish and gel on enamel erosion.

Science.gov (United States)

De Carvalho Filho, Antonio Carlos Belfort; Sanches, Roberto Pizarro; Martin, Airton Abrahão; Do Espírito Santo, Ana Maria; Soares, Luís Eduardo Silva

2011-09-01

Dental erosion is a risk factor for dental health, introduced by today's lifestyle. Topical fluoride applications in the form of varnishes and gel may lead to deposition of fluoride on enamel. This in vitro study aimed to evaluate the effect of two fluoride varnishes and one fluoride gel on the dissolution of bovine enamel by acids. Enamel samples (72) were divided (n = 8): artificial saliva (control-G1), Pepsi Twist® (G2), orange juice (G3), Duraphat® + Pepsi Twist® (G4), Duraphat® + orange juice (G5), Duofluorid® + Pepsi Twist® (G6), Duofluorid® + orange juice (G7), fluoride gel + Pepsi Twist® (G8), and fluoride gel + orange juice (G9). Fluoride gel was applied for 4 min and the varnishes were applied and removed after 6 h. The samples were submitted to six cycles (demineralization: Pepsi Twist® or orange juice, 10 min; remineralization: saliva, 1 h). Samples were analyzed by energy-dispersive X-ray fluorescence (144 line-scanning). The amount of Ca and P decreased significantly in the samples of G2 and G3, and the Ca/P ratio decreased in G3. Mineral gain (Ca) was greater in G9 samples than in G4 > G3 > G5 > G1, and (P) greater in G7 samples than in G9 > G4-6 > G2-3. The protective effect of Duofluorid® was significantly lower than fluoride gel against orange juice. The fluoride varnishes can interfere positively with the dissolution of dental enamel in the presence of acidic beverages. Fluoride gel showed the best protection level to extrinsic erosion with low costs. Copyright © 2010 Wiley-Liss, Inc.

Pre-Columbian alloys from the royal tombs of Sipan; energy dispersive X-ray fluorescence analysis with a portable equipment

Energy Technology Data Exchange (ETDEWEB)

Cesareo, R. [Dip. di Matematica e Fisica, Universita di Sassari, via Vienna 2, 07100, Sassari (Italy)], E-mail: cesareo@uniss.it; Calza, C.; Dos Anjos, M.; Lopes, R.T. [Nuclear Instrumentation Laboratory, COPPE, Universidade Federal do Rio de Janeiro (Brazil); Bustamante, A.; Fabian S, J. [Universidad Nacional Mayor de San Marcos, Lima (Peru); Alva, W.; Chero Z, L. [Museo ' Tumbas Reales de Sipan' , Lambayeque (Peru)

2010-04-15

On the north coast of present-day Peru flourished approximately between 50 and 700 AD, the Moche civilization. It was an advanced culture and the Moche were sophisticated metalsmiths, so that they are considered as the finest producers of jewels and artefacts of the region. The Moche metalworking ability was impressively demonstrated by the objects discovered by Walter Alva and coworkers in 1987, in the excavations of the 'Tumbas Reales de Sipan'. About 50 metal objects from these excavations, now at the namesake Museum, in Lambayeque, north of Peru, were analyzed with a portable equipment using energy-dispersive X-ray fluorescence. This portable equipment is mainly composed of a small size X-ray tube and a thermoelectrically cooled X-ray detector. Standard samples of gold and silver alloys were employed for quantitative analysis. It was determined that the analyzed artefacts from the 'Tumbas Reales de Sipan' are mainly composed of gold, silver and copper alloys, of gilded copper and of tumbaga, the last being a poor gold alloy enriched at the surface by depletion gilding, i.e. removing copper from the surface.

The determination of trace elements in uranium ores by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

De Villiers, W. van Z.

1983-11-01

The determination of 17 trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Rb, Sr, Th, U, V, Y, Zn and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated in this study. The determination of major elements was also necessary for the calculation of mass absorption coefficients. Initially a method was developed for the determination of the elements of interest in unmineralised silicates. Correction for absorption of radiation by the sample were made by means of mass absorption coefficients which were obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. The Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. It was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample

RADIO-QUIET AND RADIO-LOUD PULSARS: SIMILAR IN GAMMA-RAYS BUT DIFFERENT IN X-RAYS

Energy Technology Data Exchange (ETDEWEB)

Marelli, M.; Mignani, R. P.; Luca, A. De; Salvetti, D. [INAF—Istituto di Astrofisica Spaziale e Fisica Cosmica Milano, via E. Bassini 15, I-20133, Milano (Italy); Parkinson, P. M. Saz [Santa Cruz Institute for Particle Physics, Department of Physics, University of California at Santa Cruz, Santa Cruz, CA 95064 (United States); Hartog, P. R. Den [Stanford University HEPL/KIPAC, 452 Lomita Mall, Stanford, CA 94305-4085 (United States); Wolff, M. T., E-mail: marelli@iasf-milano.inaf.it [Space Science Division, Naval Research Laboratory, Washington, DC 20375-5352 (United States)

2015-04-01

We present new Chandra and XMM-Newton observations of a sample of eight radio-quiet (RQ) γ-ray pulsars detected by the Fermi Large Area Telescope. For all eight pulsars we identify the X-ray counterpart, based on the X-ray source localization and the best position obtained from γ-ray pulsar timing. For PSR J2030+4415 we found evidence for a ∼10″-long pulsar wind nebula. Our new results consolidate the work from Marelli et al. and confirm that, on average, the γ-ray-to-X-ray flux ratios (F{sub γ}/F{sub X}) of RQ pulsars are higher than for the radio-loud (RL) ones. Furthermore, while the F{sub γ}/F{sub X} distribution features a single peak for the RQ pulsars, the distribution is more dispersed for the RL ones, possibly showing two peaks. We discuss possible implications of these different distributions based on current models for pulsar X-ray emission.

X-Ray Emission Spectrometer Design with Single-Shot Pump-Probe and Resonant Excitation Capabilities

Energy Technology Data Exchange (ETDEWEB)

Spoth, Katherine; /SUNY, Buffalo /SLAC

2012-08-28

Core-level spectroscopy in the soft X-ray regime is a powerful tool for the study of chemical bonding processes. The ultrafast, ultrabright X-ray pulses generated by the Linac Coherent Light Source (LCLS) allow these reactions to be studied in greater detail than ever before. In this study, we investigated a conceptual design of a spectrometer for the LCLS with imaging in the non-dispersive direction. This would allow single-shot collection of X-ray emission spectroscopy (XES) measurements with varying laser pump X-ray probe delay or a variation of incoming X-ray energy over the illuminated area of the sample. Ray-tracing simulations were used to demonstrate how the components of the spectrometer affect its performance, allowing a determination of the optimal final design. These simulations showed that the spectrometer's non-dispersive focusing is extremely sensitive to the size of the sample footprint; the spectrometer is not able to image a footprint width larger than one millimeter with the required resolution. This is compatible with a single shot scheme that maps out the laser pump X-ray probe delay in the non-dispersive direction as well as resonant XES applications at normal incidence. However, the current capabilities of the Soft X-Ray (SXR) beamline at the LCLS do not produce the required energy range in a small enough sample footprint, hindering the single shot resonant XES application at SXR for chemical dynamics studies at surfaces. If an upgraded or future beamline at LCLS is developed with lower monochromator energy dispersion the width can be made small enough at the required energy range to be imaged by this spectrometer design.

Non-matrix corrected organic sulfur determination by energy dispersive X-ray spectroscopy for western Kentucky coals and residues

International Nuclear Information System (INIS)

Clark, C.P.; Freeman, G.B.; Hower, J.C.

1984-01-01

A method for non-matrix corrected organic sulfur analysis by energy dispersive X-ray spectroscopy has been developed using petroleum coke standards. Typically, electron beam microanalysis is a rapid, nondestructive analytical technique to quantitatively measure organic sulfur in coal. The results show good correlation to ASTM values for numerous well characterized coals with a wide range in total and pyritic sulfur content. This direct analysis is capable of reducing error commonly associated with the present ASTM method which relies on an indirect measure of organic sulfur by difference. The precision of the organic sulfur values determined in the present study is comparable to that obtained by ZAF matrix corrected microanalysis. The energy dispersive microanalysis is capable of measuring micro as well as bulk organic sulfur levels

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

International Nuclear Information System (INIS)

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

2012-01-01

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

X-ray state analysis by means of electron capture decay

Energy Technology Data Exchange (ETDEWEB)

Tamaki, Yoichi [Miyagi Univ. of Education, Sendai (Japan)

1998-01-01

K{alpha} X-ray induced by EC decay of {sup 55}Fe and {sup 71}Ge-labeled compounds were measured by wavelength dispersive X-ray spectrometer equipped position sensitive proportional detector. In both nuclides, peak energies of K{alpha}{sub 2} X-rays are lower (-0.4 - -0.6 eV) than those of Mn and Ga compounds by photoionization. It is thought that the causes of these differences are intensity of high energy satellite peaks by shake up process. (author)

On-axis microscopes for the inelastic x-ray scattering beamline at NSLS-II

Energy Technology Data Exchange (ETDEWEB)

Gofron, K. J., E-mail: kgofron@bnl.gov; Cai, Y. Q.; Coburn, D. S.; Antonelli, S.; Suvorov, A. [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY 11973 (United States); Flores, J. [Department of Physics and Astronomy, Stony Brook University, NY 11794 (United States)

2016-07-27

A novel on-axis X-ray microscope with 3 µm resolution, 3x magnification, and a working distance of 600 mm for in-situ sample alignment and X-ray beam visualization for the Inelastic X-ray Scattering (IXS) beamline at NSLS-II is presented. The microscope uses reflective optics, which minimizes dispersion, and allows imaging from Ultraviolet (UV) to Infrared (IR) with specifically chosen objective components (coatings, etc.). Additionally, a portable high resolution X-ray microscope for KB mirror alignment and X-ray beam characterization was developed.

Direct analysis of plutonium metal for gallium, iron, and nickel by energy dispersive x-ray spectrometry

International Nuclear Information System (INIS)

Bramlet, H.L.; Doyle, J.H.

1981-01-01

An x-ray secondary target method for routine determination of gallium, iron, and nickel in plutonium metal is described that has significant advantages over wet chemical analysis. Coupons requiring minimal preparation for analysis are produced as a breakaway tab on the plutonium ingot. All three elements are determined on the same coupon. Gallium is determined using an arsenic secondary target followed by iron and nickel using a zinc target. The analysis times are 5 minutes for gallium and 15 minutes for the combined iron and nickel. The method of analysis was evaluated in the range of from 0.5 to 1.5% gallium. Iron was investigated over the range of 67 to 3000 ppM and nickel from 64 to 110 ppM

The Characterisation of Settled Dust by Scanning Electron Microscopy and Energy Dispersive X-ray Analysis

International Nuclear Information System (INIS)

Shilton, Vaughan; Giess, Paul; Mitchell, David; Williams, Craig

2002-01-01

Settled dust has been collected inside the main foyers oft hree University buildings in Wolverhampton City Centre,U.K. Two of the three buildings are located in a street canyon used almost exclusively by heavy duty diesel vehicles. The dust was collected on adhesive carbonspectro-tabs to be in a form suitable for analysis by scanning electron microscope and energy dispersive X-ray analysis. Using these analytical techniques, individual particle analysis was undertaken for morphology and chemistry. Seasonal variations and variations due to location were observed in both the morphological measurements and chemical analysis. Many of the differences appear attributable to the influence of road traffic, in particular, the heavy duty diesel vehicles, travelling along the street canyon

Calcium detection in secretion granules of avian oviduct by scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDX)

International Nuclear Information System (INIS)

Makita, T.; Hatsuoka, M.; Sugi, Y.

1983-01-01

Secretion granules in the shell gland, isthmus, and albumin-secreting region of the hen oviduct were analyzed with WET-scanning electron microscopy (SEM) and EDX, a combination of wide-angle backscattered electron detector (BED) and energy-dispersive X-ray microanalyzer (EDX). Glutaraldehyde-fixed but unhydrated, unstained, and uncoated samples were analyzed; Ca was localized in all secretion granules in all three sections of the hen oviduct studied

Characterisation and application of a laser-based hard x-ray source

International Nuclear Information System (INIS)

Graetz, M.

1998-11-01

Hard X-rays are generated by focusing 110 fs laser pulses with intensities of about 1017 W/cm 2 onto solid metal targets. Characteristic properties of this X-ray source are the small source size, the short pulse duration and the high peak flux. The aim of the present work was to characterise this X-ray source and to demonstrate possible applications. A comparison with other X-ray sources and conventional imaging techniques is made. Characterising measurements were performed, including source size, emission spectrum, temporal behaviour, source stability and the influence of various laser parameters. The emission spectrum was measured using both energy-dispersive solid-state detectors and wavelength-dispersive crystal spectroscopy. The conversion efficiency from laser light to X-ray radiation was measured for different target materials. The laser ablation from different targets was studied. The feasibility of special imaging techniques, e.g. differential imaging and time-gated imaging, was investigated both theoretically and experimentally. Differential imaging allows for selective imaging of contrast agents, while time-gated imaging can reduce the influence of scattered radiation in X-ray imaging. Time-gated imaging was demonstrated in different imaging geometries, both for planar imaging and computed tomography imaging. Reasonable agreement between theoretically calculated values and experimental results was obtained

Characterisation and application of a laser-based hard x-ray source

Energy Technology Data Exchange (ETDEWEB)

Graetz, M

1998-11-01

Hard X-rays are generated by focusing 110 fs laser pulses with intensities of about 1017 W/cm{sup 2} onto solid metal targets. Characteristic properties of this X-ray source are the small source size, the short pulse duration and the high peak flux. The aim of the present work was to characterise this X-ray source and to demonstrate possible applications. A comparison with other X-ray sources and conventional imaging techniques is made. Characterising measurements were performed, including source size, emission spectrum, temporal behaviour, source stability and the influence of various laser parameters. The emission spectrum was measured using both energy-dispersive solid-state detectors and wavelength-dispersive crystal spectroscopy. The conversion efficiency from laser light to X-ray radiation was measured for different target materials. The laser ablation from different targets was studied. The feasibility of special imaging techniques, e.g. differential imaging and time-gated imaging, was investigated both theoretically and experimentally. Differential imaging allows for selective imaging of contrast agents, while time-gated imaging can reduce the influence of scattered radiation in X-ray imaging. Time-gated imaging was demonstrated in different imaging geometries, both for planar imaging and computed tomography imaging. Reasonable agreement between theoretically calculated values and experimental results was obtained 120 refs, figs, tabs

The comparative study of contents of zinc and lead in ore samples of Namtu-Bawdwin Mine by wet analysis, X-ray fluorescence and X-ray diffraction methods

Energy Technology Data Exchange (ETDEWEB)

Kyaw-Soe,

1990-05-01

Lead-zinc ores taken from Namtu-Bawdwin area had been analyzed by wet processes in the Department of Chemistry, 1984. These ore samples have been analyzed by energy dispersive X-ray fluorescence method in the Department of Physics and X-ray diffraction method is also used to determine elements of lead and zinc compounds in these ore samples in the University`s Research Centre. In brief, we study comparatively the contents of lead and zinc and their compounds using the methods of wet processes, X-ray fluorescence and X-ray diffraction. (author).

Micro-beam X-ray fluorescence and absorption imaging techniques at the IAEA Laboratories

International Nuclear Information System (INIS)

Wegrzynek, Dariusz; Markowicz, A.; Bamford, S.; Chinea-Cano, E.; Bogovac, M.

2005-01-01

X-ray tube based, micro-beam X-ray fluorescence scanning spectrometer has been equipped with two energy dispersive X-ray detectors. The two-detector configuration allows for simultaneous collection of X-ray fluorescence (XRF) and transmitted X-ray beam signals with a spatial resolution in the range of 10-50 μm, depending on the X-ray focussing element in use. The XRF signal is collected with a standard, liquid nitrogen cooled Si(Li) detector. The X-ray beam transmitted through the sample is acquired with a thermoelectrically cooled, silicon drift (SD) detector. The data acquisition is carried out in a fully automatic way under control of the SPECTOR-LOCATOR software. The software controls the scanning procedure and X-ray spectra acquisition during the scan. The energy dispersive X-ray spectra collected at every 'pixel' are stored for off-line processing. For selected regions of interest (ROI's), the element maps are constructed and displayed on-line. The spectrometer has been used for mapping elemental distributions and for performing 2D- and 3D-tomograpic imaging of minute objects in X-ray absorption and in X-ray fluorescence mode. A unique feature of the described system is simultaneous utilization of the two detectors, Si(Li) and SD, which adds new options for quantitative analysis and data interpretation. Examples of elemental mapping and 3D tomographic imaging as well as the advanced features of the SPECTOR-LOCATOR measurement control and data acquisition software are presented in this work

Nondestructive determination of lead, cadmium, tin, antimony, and barium in ceramic glazes by radioisotope X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Anderson, D.L.; Cunningham, W.C.

1996-01-01

Quantitation capabilities of radioisotope X-ray fluorescence spectrometry (RXRFS) for determining lead, cadmium, tin, antimony, and barium in ceramic glazes were investigated. Twenty-one air-dried glazes and 85 fired glazes on test tiles were analyzed by using 109 Cd and 57 Co excitation sources. Accurate Pb determinations, with limits of detection (LODs) of about 0.3 mg/cm 2 for 5 min counting times, were achieved by using the 75 keV Κ α1 X-ray photopeak and a Pb foil calibration procedure. Cd, Sn, Sb, and Ba concentrations were determined with LODs from about 0.5 to 1.5 mg/cm 2 . For Pb and Ba, results obtained by using absorption corrections based only on element concentrations determined by RXRFS and an iterative approach led to analytical biases of ≤4% relative to results obtained by using corrections based on known total element compositions. Biases were more severe for Cd, Sn, and Sb because lower X-ray energies were involved and sensitivities varied as a function of matrix Pb content. Pb concentrations were above LODs (1.3-40 mg/cm 2 ) in 39 of 47 fired open-quotes food-safeclose quotes glazes and in 33 of the other 38 fired glazes (0.4-39 mg/cm 2 ). 15 refs., 9 figs., 9 tabs

Study of change in dispersion and orientation of clay platelets in a polymer nanocomposite during tensile test by variostage small-angle X-ray scattering

CSIR Research Space (South Africa)

Bandyopadhyay, J

2012-04-01

Full Text Available To understand the change in dispersion and orientation of clay platelets in three-dimensional space during tensile test, neat polymer and its nanocomposite samples were studied by small- and wide-angle X-ray scattering (SWAXS). The samples after...

Analyses of Interaction Phases of U Mo Dispersion Fuel by Synchrotron X ray Diffraction

Energy Technology Data Exchange (ETDEWEB)

Kim, Woo Jeong; Nam, Ji Min; Ryu, Ho Jin; Park, Jong Man [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Herve, Palancher; Charollais, Francois [Saint Paul Lez Durance Cedex, Rhone (France); Bonnin, Anne; Honkimaeki, Veijo [Grenoble Cedex, Grenoble (France); Patrick Lemoined [Gif sur Yvette, Paris (France)

2012-10-15

Gamma phase U Mo alloys are one of the promising candidates to be used as advanced high uranium density fuel for high power research reactors due to their excellent irradiation performance. However, formation of interaction layers between the U Mo particles and Al matrix degrades the irradiation performance of U Mo dispersion fuel. One of the remedies to the interaction problem is a Si addition to the Al matrix. Recent irradiation tests have shown that the use of Al (2{approx}5wt%)Si matrices retarded the growth of interaction layers effectively during irradiation. Recently, KAERI has proposed silicide or nitride coated U Mo fuel for the minimization of the interaction layer growth. The silicide or nitride coatings are expected to act as interdiffusion barriers and their out of pile tests showed the improved diffusion barrier performances of the silicide and nitride layers. In order to characterize constituent phases in the coated layers on U Mo particles and the interaction layers of coated U Mo particle dispersed fuel, synchrotron X ray diffraction experiments have been performed at the ESRF (European Synchrotron Radiation Facility), France as a KAERI CEA cooperation program.

Study of soil aggregate breakdown dynamics under low dispersive ultrasonic energies with sedimentation and X-ray attenuation

Science.gov (United States)

Schomakers, Jasmin; Zehetner, Franz; Mentler, Axel; Ottner, Franz; Mayer, Herwig

2015-10-01

It has been increasingly recognized that soil organic matter stabilization is strongly controlled by physical binding within soil aggregates. It is therefore essential to measure soil aggregate stability reliably over a wide range of disruptive energies and different aggregate sizes. To this end, we tested highaccuracy ultrasonic dispersion in combination with subsequent sedimentation and X-ray attenuation. Three arable topsoils (notillage) from Central Europe were subjected to ultrasound at four different specific energy levels: 0.5, 6.7, 100 and 500 J cm-3, and the resulting suspensions were analyzed for aggregate size distribution by wet sieving (2 000-63 μm) and sedimentation/X-ray attenuation (63-2 μm). The combination of wet sieving and sedimentation technique allowed for a continuous analysis, at high resolution, of soil aggregate breakdown dynamics after defined energy inputs. Our results show that aggregate size distribution strongly varied with sonication energy input and soil type. The strongest effects were observed in the range of low specific energies (aggregate stability and release of soil organic matter upon aggregate breakdown.

Study of soil aggregate breakdown dynamics under low dispersive ultrasonic energies with sedimentation and X-ray attenuation**

Science.gov (United States)

Schomakers, Jasmin; Zehetner, Franz; Mentler, Axel; Ottner, Franz; Mayer, Herwig

2016-01-01

It has been increasingly recognized that soil organic matter stabilization is strongly controlled by physical binding within soil aggregates. It is therefore essential to measure soil aggregate stability reliably over a wide range of disruptive energies and different aggregate sizes. To this end, we tested high-accuracy ultrasonic dispersion in combination with subsequent sedimentation and X-ray attenuation. Three arable topsoils (notillage) from Central Europe were subjected to ultrasound at four different specific energy levels: 0.5, 6.7, 100 and 500 J cm−3, and the resulting suspensions were analyzed for aggregate size distribution by wet sieving (2 000-63 μm) and sedimentation/X-ray attenuation (63-2 μm). The combination of wet sieving and sedimentation technique allowed for a continuous analysis, at high resolution, of soil aggregate breakdown dynamics after defined energy inputs. Our results show that aggregate size distribution strongly varied with sonication energy input and soil type. The strongest effects were observed in the range of low specific energies (aggregate stability and release of soil organic matter upon aggregate breakdown. PMID:27099408

Visible/IR light and x-rays in femtosecond synchronism from an x-ray free-electron laser

International Nuclear Information System (INIS)

Adams, B. A.; Experimental Facilities Division

2005-01-01

A way is proposed to obtain pulses of visible/infrared light in femtosecond synchronism with x-rays from an x-ray free-electron laser (XFEL), using the recently proposed emittance-slicing technique. In an XFEL undulator, only the short section of an electron bunch whose emittance is left unchanged by the slicing will emit intense coherent x-rays in the XFEL undulator. At the same time, the bunch emits highly collimated transition undulator radiation (TUR) into a cone whose opening angle is the reciprocal relativisticity parameter gamma. Due to the variation of the transverse momentum induced by the emittance slicing, the effective number of charges contributing to the TUR varies along the bunch, and is higher in the sliced-out part that emits the coherent x-rays. As with coherent synchrotron radiation (CSR), the TUR is thus coherently enhanced (CTUR) at near-infrared wavelengths. Coming from the same part of the bunch the CTUR and the coherent x-rays are perfectly synchronized to each other. Because both types of radiation are generated in the long straight XFEL undulator, there are no dispersion effects that might induce a timing jitter. With typical XFEL parameters, the energy content of the single optical cycle of near-IR CTUR light is about 100 Nano-Joule, which is quite sufficient for most pump-probe experiments

A critical evaluation of quantitative and qualitative analysis by means of energy-dispersive X-ray measurement in a scanning electron microscope

International Nuclear Information System (INIS)

Blum, F.

1978-12-01

The bombardment of solids in the scanning electron microscope (SEM) by means of energetic electrons results in the generation and emission of various signals that carry information about the characteristics of the target. Those signals which are related to the present context, e.g. the secondary and backscattered electrons as well as the characteristic and continuous X-radiation, are discussed. The brief description of the SEM and the energy dispersive X-ray (EDX) spectrometer is followed by a discussion of various obstacles affecting the reliability of X-ray intensity measurements and data reduction procedures. The observed relative X-ray intensities from pure elements were determined as a function of the atomic number. These functional dependence curves, which were established under standard conditions, served as reliable reference data for the purpose of quantitative corrections. The performance limits of a typical SEM-EDX analytical system were assessed by analysing quantitatively various types of standard reference materials and inhomogeneous samples. A brief discussion of the X-ray source is given in order to estimate whether the recorded X-ray intensities are representative of the electron bombarded areas. This is of importance when microanalyses are performed on inclusions or near phase boundaries. The use of oxide glasses which are suitable to evaluate and interrelative SEM-EDX systems is discussed. The analysis of metal alloys, which developed exaggerated surface topography when sputtered in an ion microprobe mass analyser or glow discharge lamp, is presented as a typical example for the investigation of rough-surface samples [af

Wavelength Dispersive X-ray Fluorescence Analysis of Actinides in Dissolved Nuclear Fuels

Energy Technology Data Exchange (ETDEWEB)

O' Hara, David [Parallax Research, Inc., Tallahassee, FL (United States)

2015-10-15

There is an urgent need for an instrument that can quickly measure the concentration of Plutonium and other Actinides mixed with Uranium in liquids containing dissolved spent fuel rods. Parallax Research, Inc. proposes to develop an x-ray spectrometer capable of measuring U, Np and Pu in dissolved nuclear fuel rod material to less than 10 ppm levels to aid in material process control for these nuclear materials. Due to system noise produced by high radioactivity, previous x-ray spectrometers were not capable of low level measurements but the system Parallax proposed has no direct path for undesired radiation to get to the detector and the detector in the proposed device is well shielded from scatter and has very low dark current. In addition, the proposed spectrometer could measure these three elements simultaneously, also measuring background positions with an energy resolution of roughly 100 eV making it possible to see a small amount of Pu that would be hidden under the tail of the U peak in energy dispersive spectrometers. Another nearly identical spectrometer could be used to target Am and Cm if necessary. The proposed spectrometer needs only a tiny sample of roughly 1 micro-liter (1 mm³) and the measurement can be done with the liquid flowing in a radiation and chemical immune quartz capillary protected by a stainless steel rod making it possible to continuously monitor the liquid or to use a capillary manifold to measure other liquid streams. Unlike other methods such as mass spectroscopy where the sample must be taken to a remote facility and might take days for turn-around, the proposed measurement should take less than an hour. This spectrometer could enable near real-time measurement of U, Pu and Np in dilute dissolved spent nuclear fuel rod streams.

Bulk substrate porosity verification by applying Monte Carlo modeling and Castaing's formula using energy-dispersive x-rays

Science.gov (United States)

Yung, Lai Chin; Fei, Cheong Choke; Mandeep, Jit Singh; Amin, Nowshad; Lai, Khin Wee

2015-11-01

The leadframe fabrication process normally involves additional thin-metal layer plating on the bulk copper substrate surface for wire bonding purposes. Silver, tin, and copper flakes are commonly adopted as plating materials. It is critical to assess the density of the plated metal layer, and in particular to look for porosity or voids underneath the layer, which may reduce the reliability during high-temperature stress. A fast, reliable inspection technique is needed to assess the porosity or void weakness. To this end, the characteristics of x-rays generated from bulk samples were examined using an energy-dispersive x-ray (EDX) detector to examine the porosity percentage. Monte Carlo modeling was integrated with Castaing's formula to verify the integrity of the experimental data. Samples with different porosity percentages were considered to test the correlation between the intensity of the collected x-ray signal and the material density. To further verify the integrity of the model, conventional cross-sectional samples were also taken to observe the porosity percentage using Image J software measurement. A breakthrough in bulk substrate assessment was achieved by applying EDX for the first time to nonelemental analysis. The experimental data showed that the EDX features were not only useful for elemental analysis, but also applicable to thin-film metal layer thickness measurement and bulk material density determination. A detailed experiment was conducted using EDX to assess the plating metal layer and bulk material porosity.

Using Synchrotron-based X-ray Absorption Spectrometry to Identify the Arsenic Chemical Forms in Mine Waste Materials

International Nuclear Information System (INIS)

Matanitobua, Vitukawalu P.; Noller, Barry N.; Chiswell, Barry; Ng, Jack C.; Bruce, Scott L.; Huang, Daphne; Riley, Mark; Harris, Hugh H.

2007-01-01

X-ray Absorption Near Edge Spectroscopy (XANES) gives arsenic form directly in the solid phase and has lower detection limits than extraction techniques. An important and common application of XANES is to use the shift of the edge position to determine the valence state. XANES speciation analysis is based on fitting linear combinations of known spectra from model compounds to determine the ratios of valence states and/or phases present. As(V)/As(III) ratios were determined for various Australian mine waste samples and dispersed mine waste samples from river/creek sediments in Vatukoula, Fiji

Surface characterization of selected polymer thin films by total-reflection x-ray fluorescence spectroscopy and x-ray reflectivity

International Nuclear Information System (INIS)

Innis, Vallerie Ann A.

2006-01-01

Development of available x-ray characterizations tools for grazing incidence techniques was done to be able to probe nano-size thin films. Alignment of a Philips x-ray powder diffractometer was improved to let it perform as an x-ray reflectometer. X-ray reflectometry was coupled with total-reflection x-ray fluorescence spectroscopy. Evaluation of the performance of this grazing incidence techniques was done by preparing polymer thin films of carboxymethylcellulose, carrageenan and polyvinylpyrrolidone (PVP). The thickness of the films were varied by varying the process parameters such as concentration, spin speed and spin time. Angle-dispersive total-reflection x-ray fluorescence spectroscopy profiles of three films showed film formation only in carrageenan and PVP. For both carrageenan and PVP, an increase in concentration yielded a corresponding increase in intensity of the fluorescent or scattered peaks. XRR profiles of carrageenan thin films yielded a mean value for the critical angle close to quartz substrate. Thickness measurements of the prepared carrageenan thin films showed that concentration was the main determinant for final film thickness over the other process parameters. Sulfur fluorescent intensity derived from the TXRF measurement showed a linear relationship with the measured thickness by XRR. For PVP, measured critical angle is lower than quartz. Poor adhesion of the polymer onto the substrate yielded a limited number of thickness measurements made from the XRR profiles. (Author)

X-ray filter for x-ray powder diffraction

Science.gov (United States)

Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.; Dooryhee, Eric; Ghose, Sanjit

2018-01-23

Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and walls defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.

Scanning electron microscope/energy dispersive x ray analysis of impact residues on LDEF tray clamps

Science.gov (United States)

Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

1992-01-01

To better understand the nature of particulates in low-Earth orbit (LEO), and their effects on spacecraft hardware, we are analyzing residues found in impacts on the Long Duration Exposure Facility (LDEF) tray clamps. LDEF experiment trays were held in place by 6 to 8 chromic-anodized aluminum (6061-T6) clamps that were fastened to the spacecraft frame using three stainless steel hex bolts. Each clamp exposed an area of approximately 58 sq cm (4.8 cm x 12.7 cm x .45 cm, minus the bolt coverage). Some 337 out of 774 LDEF tray clamps were archived at JSC and are available through the Meteoroid & Debris Special Investigation Group (M&D SIG). Optical scanning of clamps, starting with Bay/Row A01 and working toward H25, is being conducted at JSC to locate and document impacts as small as 40 microns. These impacts are then inspected by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis (SEM/EDXA) to select those features which contain appreciable impact residue material. Based upon the composition of projectile remnants, and using criteria developed at JSC, we have made a preliminary discrimination between micrometeoroid and space debris residue-containing impact features. Presently, 13 impacts containing significant amounts of unmelted and semi-melted micrometeoritic residues were forwarded to Centre National d'Etudes Spatiales (CNES) in France. At the CNES facilities, the upgraded impacts were analyzed using a JEOL T330A SEM equipped with a NORAN Instruments, Voyager X-ray Analyzer. All residues were quantitatively characterized by composition (including oxygen and carbon) to help understand interplanetary dust as possibly being derived from comets and asteroids.

Advanced β-ray-induced X-ray spectrometry for non-destructive measurement of tritium retained in fusion related materials

Energy Technology Data Exchange (ETDEWEB)

Matsuyama, Masao, E-mail: matsu3h@ctg.u-toyama.ac.jp; Abe, Shinsuke

2016-11-01

Highlights: • A new measurement system to measure low-Z elements such as C and O atoms has been constructed for evaluation of tritium trapped by these elements. - Abstract: A new β-ray-induced X-ray measurement system equipped with a silicon drift detector, which was named “Advanced-BIXS”, was constructed to study in detail retention behavior of surface tritium by measurements of low energy X-rays below 1 keV such as C(K{sub α}) and O(K{sub α}) as well as high energy X-rays induced by β-rays from tritium. In this study, basic performance of the present system has been examined using various tritium-containing samples. It was seen that energy linearity, energy resolution and sensitivity were quite enough for measurements of low energy X-rays induced by β-rays. Intensity of characteristic X-rays emitted from the surface and/or bulk of a tritium-containing sample was lowered by argon used as a working gas of the Advanced-BIXS. Pressure dependence of transmittance of C(K{sub α}) and Fe(K{sub α}) was examined as examples of low and high energy X-rays, and it was able to represent by using the mass absorption coefficient in argon. It was concluded, therefore, that the present system has high potentiality for nondestructive measurements of tritium retained in surface layers and/or bulk of fusion related materials.

The determination of the C, N, O and trace element content of Triticum aestivum by activation analysis, X-ray excitation and mass spectrometry

International Nuclear Information System (INIS)

Leonhardt, J.W.; Dahn, E.; Dietze, H.J.; Freyer, K.; Geisler, M.; Hartmann, G.; Jung, K.; Schelhorn, H.

1979-01-01

The results of determinations of the C, N, O and trace element content of grains, sprouts and leaves of Triticum aestivum by means of various methods of activation analysis, X-ray excitation and mass spectrometry are presented. The C and O contents were determined by X-ray excitation; the O, N, P and Si contents were measured by NAA with 14-MeV neutrons, and the trace elements were determined by NAA with thermal neutrons. A mass-spectrometric survey analysis confirmed the results obtained by NAA. The use of neutron-induced nuclear reactions together with autoradiography enabled a representative picture to be formed of the spatial distribution in two dimensions of 14 N in biological specimens. (author)

Thermoelectrically cooled semiconductor detectors for non-destructive analysis of works of art by means of energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Cesareo, Roberto; Ettore Gigante, Giovanni; Castellano, Alfredo

1999-01-01

Thermoelectrically cooled semiconductor detectors, such as Si-PIN, Si-drift, Cd 1-x Zn x Te and HgI 2 , coupled to miniaturized low-power X-ray tubes, are well suited in portable systems for energy-dispersive X-ray fluorescence (EDXRF), analysis of archaeological samples. The Si-PIN detector is characterized by a thickness of about 300 μm, an area of about 2x3 mm 2 , an energy resolution of about 200-250 eV at 5.9 keV and an entrance window of 25-75 μm. The Si-drift detector has approximately the same area and thickness, but an energy resolution of 155 eV at 5.9 keV. The efficiency of these detectors is around 100% from 4 to 10 keV, and then decreases versus energy, reaching ∼9% at 30 keV. Coupled to a miniaturized 10 kV, 0.1 mA, Ca-anode or to a miniaturized 30 kV, 0.1 mA, W-anode X-ray tubes, portable systems can be constructed, which are able to analyse K-lines of elements up to about silver, and L-lines of heavy elements. The Cd 1-x Zn x Te detector has an area of 4 mm 2 and a thickness of 3 mm. It has an energy resolution of about 300 eV at 5.9 keV, and an efficiency of 100% over the whole range of X-rays. Finally the HgI 2 detector has an efficiency of about 100% in the whole range of X-rays, and an energy resolution of about 200 eV at 5.9 keV. Coupled to a small 50-60 kV, 1 mA, W-anode X-ray tube, portable systems can be constructed, for the analysis of practically all elements. These systems were applied to analysis in the field of archaeometry and in all applications for which portable systems are needed or at least useful (for example X-ray transmission measurements, X-ray microtomography and so on). Results of in-field use of these detectors and a comparison among these room temperature detectors in relation to concrete applications are presented. More specifically, concerning EDXRF analysis, ancient gold samples were analysed in Rome, in Mexico City and in Milan, ancient bronzes in Sassari, in Bologna, in Chieti and in Naples, and sulfur (due to

Determination of silver in ancient coins by X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Pairatana, C.

1976-01-01

45 coins of late Ayudhaya and Bangkok periods was analyzed quantitatively by x-ray fluorescence technique using radioisotopic sources Pm - 147/A1 and Am - 241. The fluorescence x-rays were detected by Lithium drifted silicon detector and 1024 channels pulse height analyzer. The procedure was laid a stress on non-destructive methods which could be utilized for analysing various kinds of antiquities and work of arts such as metals, alloys, pottery, ceramics, paper, textile, wood etc

Characterization of sediments laid on Solimoes/Amazonas river flood plains, using energy dispersive X-ray fluorescence technique

International Nuclear Information System (INIS)

Carneiro, Ana E.V.; Nascimento Filho, Virgilio F. do

1997-01-01

This paper proposes sediment analysis with high light elements fraction using dispersive energy X-ray fluorescence technique with radioisotopic excitation, The proposed procedure is based on the Fundamental Parameters for analytical elements (Z ≥ 13) evaluation, and coherent and incoherent scattered radiation for quantification of the light fraction of the matrix (Z < 13). Laid sediments samples on Solimoes/Amazonas river flood plains were analyzed, determining simultaneously the Al, Si, K, Ca, Ti, Fe, Sc, V, Mn, Cu, Zn, Rb, Sr and Zr element concentrations, thus allowing chemical characterization and spatial variability, and some mineralogical and weathering sediments aspects. (author). 15 refs., 11 tabs

Time-resolved and position-resolved X-ray spectrometry with a pixelated detector

Energy Technology Data Exchange (ETDEWEB)

Sievers, Peter

2012-12-07

show a good agreement. Up to now the measurements of impinging spectra with a Timepix detector have been performed in radiation fields with a relatively high fluence. To cope with the requirement of measuring in radiation fields with a low fluence, there had to be changes in the method of analysis compared to those performed formerly. An important improvement in this context was the employment of the Bayesian deconvolution method. The spectra reconstructed with this method were then compared to the results of two different and established detection systems. Firstly, the shape of the deconvolved spectrum was compared to the one measured with a hpGe detector. Secondly, the calculated value of the kerma rate was compared to the one measured with an ionization chamber. This gave an estimate on the correctness of the absolute number of photons. Both comparisons have shown a good agreement and thus I was able to validate that the method delivers precise results. Compared to the formerly used spectrum-stripping method the Bayesian deconvolution turned out to be very stable and reliable. This robustness of the deconvolution method and the development of a pixel-by-pixel energy calibration were the keys towards position-resolved spectrometry. With such a precise energy calibration the energy resolution was enhanced by up to 45%. This improved accuracy in the measurement has been very demanding on the improvements of the simulation of the response matrix needed for deconvolution. Both this enhanced simulation and a pixel-by-pixel calibrated detector opened the possibility of measuring the anode heel effect. Not only the relative angular dependency of the spectrum emitted but also the change in the absolute photon fluence were measured. Furthermore, it is possible to even use small ROIs down to 4x4 pixels to evaluate a spectrum. This was then applied for the spectrometry of small focal spots of a miniature X-ray source used in therapeutics. Furthermore, the robustness and the

Time-resolved and position-resolved X-ray spectrometry with a pixelated detector

International Nuclear Information System (INIS)

Sievers, Peter

2012-01-01

show a good agreement. Up to now the measurements of impinging spectra with a Timepix detector have been performed in radiation fields with a relatively high fluence. To cope with the requirement of measuring in radiation fields with a low fluence, there had to be changes in the method of analysis compared to those performed formerly. An important improvement in this context was the employment of the Bayesian deconvolution method. The spectra reconstructed with this method were then compared to the results of two different and established detection systems. Firstly, the shape of the deconvolved spectrum was compared to the one measured with a hpGe detector. Secondly, the calculated value of the kerma rate was compared to the one measured with an ionization chamber. This gave an estimate on the correctness of the absolute number of photons. Both comparisons have shown a good agreement and thus I was able to validate that the method delivers precise results. Compared to the formerly used spectrum-stripping method the Bayesian deconvolution turned out to be very stable and reliable. This robustness of the deconvolution method and the development of a pixel-by-pixel energy calibration were the keys towards position-resolved spectrometry. With such a precise energy calibration the energy resolution was enhanced by up to 45%. This improved accuracy in the measurement has been very demanding on the improvements of the simulation of the response matrix needed for deconvolution. Both this enhanced simulation and a pixel-by-pixel calibrated detector opened the possibility of measuring the anode heel effect. Not only the relative angular dependency of the spectrum emitted but also the change in the absolute photon fluence were measured. Furthermore, it is possible to even use small ROIs down to 4x4 pixels to evaluate a spectrum. This was then applied for the spectrometry of small focal spots of a miniature X-ray source used in therapeutics. Furthermore, the robustness and the

Improvements on Low Level Activity Gamma Measurements and X-ray Spectrometry at the CEA-MADERE Measurement Platform

Directory of Open Access Journals (Sweden)

Sergeyeva Victoria

2016-01-01

Full Text Available The CEA MADERE platform (Measurement Applied to DosimEtry in REactors is a part of the Instrumentation Sensors and Dosimetry Laboratory (LDCI. This facility is dedicated to the specific activity measurements of solid and radioactive samples using Gamma and X-ray spectrometry. MADERE is a high-performance facility devoted to neutron dosimetry for experimental programs performed in CEA and for the irradiation surveillance programmes of PWR vessels. The MADERE platform is engaged in a continuous improvement process. Recently, two High Efficiency diodes have been integrated to the MADERE platform in order to manage the accurate low level activity measurements (few Bq per sample. This new equipment provides a good level of efficiency over the energy range from 60 keV to 2 MeV. The background continuum is reduced due to the use of a Ultra Low Background (ULB lead shielding. Relative and absolute X-ray measurement techniques have been improved in order to facilitate absolute rhodium activity measurement (Rh103m on solid samples. Additional efforts have been made to increase the accuracy of the relative niobium (Nb93m activity measurement technique. The way of setting up an absolute measurement method for niobium is under investigation. After a presentation of the MADERE's measurement devices, this paper focuses on the technological options taken into account for the design of high efficiency measurement devices. Then, studies performed on X-ray measurement techniques are presented. Some details about the calculation of uncertainties and correction factors are also mentioned. Finally, future research and development axes are exposed.

Analytical electron microscope based on scanning transmission electron microscope with wavelength dispersive x-ray spectroscopy to realize highly sensitive elemental imaging especially for light elements

International Nuclear Information System (INIS)

Koguchi, Masanari; Tsuneta, Ruriko; Anan, Yoshihiro; Nakamae, Koji

2017-01-01

An analytical electron microscope based on the scanning transmission electron microscope with wavelength dispersive x-ray spectroscopy (STEM-WDX) to realize highly sensitive elemental imaging especially for light elements has been developed. In this study, a large-solid-angle multi-capillary x-rays lens with a focal length of 5 mm, long-time data acquisition (e.g. longer than 26 h), and a drift-free system made it possible to visualize boron-dopant images in a Si substrate at a detection limit of 0.2 atomic percent. (paper)

Progress in x-ray microanalysis in the analytical electron microscope

International Nuclear Information System (INIS)

Williams, D.B.

1987-01-01

Analytical electron microscopes (AEM) consisting of x-ray energy dispersive spectrometers (EDS) interfaced to scanning transmission electron microscopes have been available for more than a decade. During that time, progress towards reaching the fundamental limits of the technique has been slow. The progress of x-ray microanalysis in AEM is examined in terms of x-ray detector technology; the EDS/AEM interface; accuracy of microanalysis; and spatial resolution and detectability limits. X-ray microanalysis in the AEM has substantial room for improvement in terms of the interface between the detector and the microscope. Advances in microscope design and software should permit 10nm resolution with detectability limits approaching 0.01wt percent. 16 refs., 2 figs., 1 tab

Bibliographical study on the high-purity germanium radiation detectors used in gamma and X spectrometry

International Nuclear Information System (INIS)

Bornand, Bernard; Friant, Alain

1979-03-01

The germanium or silicon lithium-drifted detectors, Ge(Li) or Si(Li), and high-purity germanium detectors, HP Ge (impurity concentration approximately 10 10 cm -3 ), are the most commonly used at the present time as gamma and X-ray spectrometers. The HP Ge detectors for which room temperature storage is the main characteristic can be obtained with a large volume and a thin window, and are used as the Ge(Li) in γ ray spectrometry or the Si(Li) in X-ray spectrometry. This publication reviews issues from 1974 to 1978 on the state of the art and applications of the HP Ge semiconductor detectors. 101 bibliographical notices with French summaries are presented. An index for authors, documents and periodicals, and subjects is included [fr

Native State Mass Spectrometry, Surface Plasmon Resonance, and X-ray Crystallography Correlate Strongly as a Fragment Screening Combination.

Science.gov (United States)

Woods, Lucy A; Dolezal, Olan; Ren, Bin; Ryan, John H; Peat, Thomas S; Poulsen, Sally-Ann

2016-03-10

Fragment-based drug discovery (FBDD) is contingent on the development of analytical methods to identify weak protein-fragment noncovalent interactions. Herein we have combined an underutilized fragment screening method, native state mass spectrometry, together with two proven and popular fragment screening methods, surface plasmon resonance and X-ray crystallography, in a fragment screening campaign against human carbonic anhydrase II (CA II). In an initial fragment screen against a 720-member fragment library (the "CSIRO Fragment Library") seven CA II binding fragments, including a selection of nonclassical CA II binding chemotypes, were identified. A further 70 compounds that comprised the initial hit chemotypes were subsequently sourced from the full CSIRO compound collection and screened. The fragment results were extremely well correlated across the three methods. Our findings demonstrate that there is a tremendous opportunity to apply native state mass spectrometry as a complementary fragment screening method to accelerate drug discovery.

Iron overload of human colon adenocarcinoma cells studied by synchrotron-based X-ray techniques

NARCIS (Netherlands)

Mihucz, Victor G.; Meirer, Florian; Polgári, Zsófia; Réti, Andrea; Pepponi, Giancarlo; Ingerle, Dieter; Szoboszlai, Norbert; Streli, Christina

2016-01-01

Fast- and slow-proliferating human adenocarcinoma colorectal cells, HT-29 and HCA-7, respectively, overloaded with transferrin (Tf), Fe(III) citrate, Fe(III) chloride and Fe(II) sulfate were studied by synchrotron radiation total-reflection X-ray spectrometry (TXRF), TXRF-X-ray absorption near edge

Synchrotron X-ray fluorescence analysis in environmental and earth sciences

Directory of Open Access Journals (Sweden)

Adams F.

2010-12-01

Full Text Available Compared to other microscopic analytical tools X-ray microscopy techniques have the advantage that the large penetration depth of X-rays in matter allows one to investigate the interior of an object without destructive sample preparation. In combination with X-ray fluorescence tomography, analytical information from inside of a specimen can be obtained. Different X-ray analytical techniques can be used to produce contrast, X-ray absorption, fluorescence, and diffraction, to yield chemical, elemental, and structural information about the sample. Scanning microscopy on the basis of various lens systems in synchrotron radiation sources provides a routine spatial resolution of now about 100 nanometer but in the foreseeable future a 10–20 nanometer spatial resolution can be expected. X-ray absorption spectrometry can also provide chemical (speciation information on the sample. All this makes X-ray microscopy attractive to many fields of science. In this paper the techniques are briefly reviewed and a number of applications in the earth, planetary and cosmos sciences are illustrated with state-of-the art examples, while applications in the environmental sciences and biology are also briefly discussed.

The First Non-Dispersive High-Resolution Spectroscopy of an X-ray-bright Galaxy Cluster

Science.gov (United States)

Yamaguchi, Hiroya; Hitomi Collaboration

2018-06-01

The Hitomi X-ray Observatory was equipped with the Soft X-ray Spectrometer (SXS), an X-ray microcalorimeter that achieved an energy resolution of 5 eV (@0.5-10 keV) for extended objects. This offered an unprecedented benchmark of atomic modeling and database for hot collisional plasmas, revealing both successes and challenges in the current atomic codes that are widely used by the X-ray astronomy community. I will review the Hitomi observations of the brightest part of the Perseus Cluster, whose X-ray spectrum is dominated by thermal emission from the intra-cluster medium (ICM). The SXS successfully measured the turbulent velocities and metal abundances of the ICM, which radically altered our understanding of the dynamics and chemical enrichment in this object. At the same time, the high-resolution X-ray data led to significant improvement in the atomic models, such as AtomDB and SPEX -- I will briefly overview how this improvement was made. Nevertheless, there are still significant discrepancies among the public atomic models, causing systematic uncertainties in measurements of the temperature, abundance, and degree of the resonance scattering. Requirements for future improvements will be summarized in this context.

An Energy Dispersive X-ray Spectroscopy Analysis of Elemental Changes of a Persimmon Phytobezoar Dissolved in Coca-Cola.

Science.gov (United States)

Iwamuro, Masaya; Urata, Haruo; Higashi, Reiji; Nakagawa, Masahiro; Ishikawa, Shin; Shiraha, Hidenori; Okada, Hiroyuki

To investigate the mechanism of phytobezoar dissolution by Coca-Cola(®), persimmon phytobezoar pieces removed from a 60-year-old Japanese woman were analyzed by energy dispersive X-ray spectroscopy. The amount of calcium significantly decreased after dissolution treatment using Coca-Cola(®), suggesting a potential contribution of calcium to dissolution mechanisms. Moreover, immersion in Coca-Cola(®) for 120 hours on the exterior surface revealed that Coca-Cola(®) did not permeate persimmon phytobezoars. This is the first study to investigate the mechanisms of persimmon phytobezoar permeability and dissolution induced by Coca-Cola(®).

A new life for the wavelength-dispersive X-ray spectrometer (WDS): incorporation of a silicon drift detector into the WDS for improved quantification and X-ray mapping

Science.gov (United States)

Wuhrer, R.; Moran, K.

2018-01-01

The wavelength-dispersive X-ray spectrometer (WDS) has been around for a long time and the design has not changed much since its original development. The electron microprobe operator using WDS has to be meticulous in monitoring items such as gas flow, gas purity, gas pressure, noise levels of baseline and window, gas flow proportional counter (GFPC) voltage levels, count rate suppression, anode wire contamination and other detector parameters. Recent development and improvements of silicon drift detectors (SDD’s) has allowed the incorporation of a SDD as the X-ray detector in place of the proportional counter (PC) and/or gas flow proportional counter (GFPC). This allows minimal mechanical alteration and no loss of movement range. The superiority of a WDS with a SDD, referred to as SD-WDS, is easily seen once in operation. The SD-WDS removes many artefacts including the worse of all high order diffraction, thus allowing more accurate analysis. The incorporation of the SDD has been found to improve the light and mid element range and consequently improving the detection limit for these elements. It is also possible to obtain much more reliable results at high count rates with almost no change in resolution, gain and zero-peak characteristics of the energy spectrum.

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-06-15

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

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

International Nuclear Information System (INIS)

Pessanha, Sofia; Carvalho, Maria Luisa; Becker, Maria; Bohlen, Alex von

2010-01-01

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

The performance of the curved grid gas proportional scintillation counter in X-ray spectrometry

International Nuclear Information System (INIS)

Santos, J.M.F. dos; Bento, A.C.S.S.M.; Conde, C.A.N.

1994-01-01

The performance of a curved grid gas proportional scintillation counter filled with xenon at 1100 mbar and having a 25 mm diameter window is evaluated for X-rays in the 1-11 keV energy range. Energy resolutions of 8.0% were obtained for a 5.9 keV parallel X-ray beam entering the detector through the full size window. The variation of the energy resolution with the X-ray energy is studied and X-ray fluorescence spectra for samples like industrial coal, painted porcelain and car lubrication oil, are presented. (orig.)

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

International Nuclear Information System (INIS)

YangDai, Tianyi; Zhang, Li

2016-01-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Energy Technology Data Exchange (ETDEWEB)

YangDai, Tianyi [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China); Zhang, Li, E-mail: zhangli@nuctech.com [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China)

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Science.gov (United States)

YangDai, Tianyi; Zhang, Li

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

A study on the determination of Ca/P molar ratio in calcium-hydroxyapatite by alpha excited x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Mizumoto, Yoshihiko; Iwata, Shiro.

1979-01-01

Nondestructive powdery calcium-hydroxyapatite (HAp) target was prepared by electrodeposition method. The powdery HAp was deposited on the copper electrode plate of cathode in the electrodeposition solution such as ethyl alcohol, methyl alcohol, etc. The experiments were carried out as functions of different electrodeposition solution, ethyl alcohol concentration, distance between anode and cathode, electrodeposition time and HAp amount added in bath, and distribution of HAp on the copper electrode plate obtained from each experiment was investigated by alpha excited X-ray fluorescence analysis. Ca/P molar ratio of thin HAp target prepared with this method was determined by alpha excited X-ray fluorescence spectrometry. The nondestructive HAp targets of thickness in the range of 5 mu g/cm 2 to 10 mg/cm 2 were easily prepared with comparatively simple apparatus. The HAp on the copper electrode plate was uniform thickness over 15 x 20 mm copper plate within 5%. The Ca/P molar ratio of HAp was 1.64 +- 0.05, which agreed well with stoichiometric value of 1.67 in HAp within standard deviation. (author)

Effects of gamma-ray irradiation on the optical properties of amorphous Se100-xHgx thin films

Science.gov (United States)

Ahmad, Shabir; Islam, Shama; Nasir, Mohd.; Asokan, K.; Zulfequar, M.

2018-06-01

In this study, the thermal quenching technique was employed to prepare bulk samples of Se100-xHgx (x = 0, 5, 10, 15). Thin films with a thickness of ∼250 nm were deposited on glass substrates using the thermal evaporation technique. These films were irradiated with gamma rays at doses of 25-100 kGy. The elemental compositions of the as-deposited thin films were confirmed by energy dispersive X-ray analysis and Rutherford backscattering spectrometry. X-ray diffraction analysis confirmed the crystalline nature of these thin films upto the dose of 75 kGy. Fourier transform-infrared spectroscopy showed that the concentration of defects decreased after gamma irradiation. Microstructural analysis by field emission scanning electron microscopy indicated that the grain size increases after irradiation. Optical study based on spectrophotometry showed that the optical band gap values of these films increase after the addition of Hg whereas they decrease after gamma irradiation. We found that the absorption coefficient increases with doses up to 75 kGy but decreases at higher doses. These remarkable shifts in the optical band gap and absorption coefficient values are interpreted in terms of the creation and annihilation of defects, which are the main effects produced by gamma irradiation.

X-Ray Absorption with Transmission X-Ray Microscopes

NARCIS (Netherlands)

de Groot, F.M.F.

2016-01-01

In this section we focus on the use of transmission X-ray microscopy (TXM) to measure the XAS spectra. In the last decade a range of soft X-ray and hard X-ray TXM microscopes have been developed, allowing the measurement of XAS spectra with 10–100 nm resolution. In the hard X-ray range the TXM

Trace-element analysis of uranium ores by x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Coetzee, P.P.; De Villiers, W.v Z.

1985-01-01

The determination of seventeen trace elements (As, Ba, Co, Cr, Cu, Mo, Nb, Ni, Pb, Sr, Th, U, V, Y, Zn, and Zr) in uranium ores by x-ray fluorescence spectrometry was investigated. For the elements with analyte lines in the vicinity of the U-L lines, large overlap corrections were necessary and only a few completely interference-free background positions were available. Consequently, the Feather and Willis method was used for determining the background intensity at the peak positions as well as mass absorption coefficients. As a result of the presence of the U-L absorption edges, both primary and secondary mass absorption coefficients had to be used for matrix corrections. Furthermore, it was observed that the background intensity in the region of the uranium lines increased with increasing uranium content of the sample, instead of the expected decrease due to the increasing mass absorption coefficient. This was attributed to the scattering of uranium lines in the spectrometer chamber. A method was developed to correct the measured intensities for this effect. The contribution from the scattering of uranium lines to the measured intensity at the various 20 positions was determined on samples with different uranium concentrations and for which the mass absorption coefficients and concentrations of the various elements were known

Synchrotron X-ray induced solution precipitation of nanoparticles

CERN Document Server

Lee, H J; Hwu, Y; Tsai, W L

2003-01-01

By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100-300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (e sub a sub q sup -), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

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

International Nuclear Information System (INIS)

Mihucz, Victor G.; Moricz, Agnes M.; Kroepfl, Krisztina; Szikora, Szilvia; Tatar, Eniko; Parra, Lue Meru Marco; Zaray, Gyula

2006-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2006-11-15

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

Chemical analysis by X-ray fluorescence, of niobium in high-strength plate steels

International Nuclear Information System (INIS)

Iozzi, F.B.; Dias, M.J.P.

1981-01-01

The use of X-ray fluorescence spectrometry in quantitative analysis of niobium in steels, as an alternative solution for optical emission spectrometry, in the rapid chemical control of steel fabrication by LD type converters, is presented. (M.C.K.) [pt

X-ray methods for the chemical characterization of atmospheric aerosols

International Nuclear Information System (INIS)

Jaklevic, J.M.; Thompson, A.C.

1981-05-01

The development and use of several x-ray methods for the chemical characterization of atmospherical aerosol particulate samples are described. These methods are based on the emission, absorption, and scattering of x-ray photons with emphasis on the optimization for the non-destructive analysis of dilute specimens. Techniques discussed include photon induced energy dispersive x-ray fluorescence, extended x-ray absorption fine structure spectroscopy using synchrotron radiation and high-rate x-ray powder diffractometry using a position-sensitive gas proportional counter. These x-ray analysis methods were applied to the measurement of the chemical compositions of size-segregated aerosol particulate samples obtained with dichotomous samplers. The advantages of the various methods for use in such measurements are described and results are presented. In many cases, the complementary nature of the analytical information obtained from the various measurements is an important factor in the characterization of the sample. For example, the multiple elemental analyses obtained from x-ray fluorescence can be used as a cross check on the major compounds observed by powder diffraction

ON NEUTRAL ABSORPTION AND SPECTRAL EVOLUTION IN X-RAY BINARIES

International Nuclear Information System (INIS)

Miller, J. M.; Cackett, E. M.; Reis, R. C.

2009-01-01

Current X-ray observatories make it possible to follow the evolution of transient and variable X-ray binaries across a broad range in luminosity and source behavior. In such studies, it can be unclear whether evolution in the low-energy portion of the spectrum should be attributed to evolution in the source, or instead to evolution in neutral photoelectric absorption. Dispersive spectrometers make it possible to address this problem. We have analyzed a small but diverse set of X-ray binaries observed with the Chandra High Energy Transmission Grating Spectrometer across a range in luminosity and different spectral states. The column density in individual photoelectric absorption edges remains constant with luminosity, both within and across source spectral states. This finding suggests that absorption in the interstellar medium strongly dominates the neutral column density observed in spectra of X-ray binaries. Consequently, evolution in the low-energy spectrum of X-ray binaries should properly be attributed to evolution in the source spectrum. We discuss our results in the context of X-ray binary spectroscopy with current and future X-ray missions.

Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

Science.gov (United States)

Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

2015-02-05

The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of radionuclide sources for excitation in energy-dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Hoffmann, P.

1986-01-01

X-ray fluorescence (XRF) analysis is in broad application in many fields of science where elemental determinations are necessary. Solid and liquid samples are analyzed by this method. Solids are introduced in thin or thick samples as melted glass, pellets, powders or as original specimen. The excitation of X-ray spectra can be performed by specific and polychromic radiation of X-ray tubes, by protons, deuterons, α-particles, heavy ions and synchrotron radiation from accelerators and by α-particles, X- and γ-rays and by bremsstrahlung generated by β - -particles from radionuclide sources. The radionuclides are devided into groups with respect to their decay mode and the energy of the emitted radiation. The broad application of radionuclides in XRF excitation is shown in examples as semi-quantitative analysis of glasses, as quantitative analysis of coarse ceramics and as quantitative determination of heavy elements (mainly actinides) in solutions. The advantages and disadvantages of radionuclide excitation in XRF analysis are discussed. (orig.) [de

An X-ray wave theory for heavily distorted crystals. 1

International Nuclear Information System (INIS)

Ohkawa, T.; Hashimoto, H.

1985-01-01

An X-ray diffraction theory is developed of monochromatic waves having spherical wave front, which is applicable to an interpretation of divergent X-ray diffraction images of crystals containing arbitral types of strain field. The theory is divided into two parts. In part I, Takagi's theory is expanded by introducing amplitude and phase correction functions and a new improved representation for the X-ray diffraction theory is given. In part II dispersion surfaces in heavily distorted crystals are discussed, and in the discussion the resonance shift functions are introduced. These formulations can lead to a complete understanding of the extinction phenomena. (author)

SEXTANT X-Ray Pulsar Navigation Demonstration: Initial On-Orbit Results

Science.gov (United States)

Mitchell, Jason W.; Winternitz, Luke B.; Hassouneh, Munther A.; Price, Samuel R.; Semper, Sean R.; Yu, Wayne H.; Ray, Paul S.; Wolf, Michael T.; Kerr, Matthew; Wood, Kent S.;

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

International Nuclear Information System (INIS)

Franca, Alana Caroline; Torres, Catarina A.M.P.; Rocha, Ana S.S.; Deniak, Valeriy; Lara, Alessandro L.; Paschuk, Sergei A.; Fernandes, Angela; Westphalen, Fernando Henrique

2013-01-01

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

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